Continuously updated synthesis method about 7170-01-6

The synthetic route of 7170-01-6 has been constantly updated, and we look forward to future research findings.

Related Products of 7170-01-6, A common heterocyclic compound, 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, molecular formula is C3H5N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

5-(3-Methyl-1H-1,2,4-triazol-1-yl)pyrazine-2-carboxylic acid A mixture of methyl 5-chloropyrazine-2-carboxylate (0.75 g), K2CO3 (1.8 g) and 3-methyl-1H-1,2,4-triazole (1.2 g) in N,N-dimethylformamide (6 mL) is heated to 100 C. overnight. Analysis of the crude mixture by LCMS shows saponified product. The product is acidified with 1N HCl and the precipitate is filtered and washed with water and diethyl ether to afford the title compound. LC (method 20): tR=1.21 min; Mass spectrum (APCI): m/z=206 [M+H]+.

The synthetic route of 7170-01-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NEUROCRINE BIOSCIENCES, INC.; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; HECKEL, Armin; HIMMELSBACH, Frank; LANGKOPF, Elke; NOSSE, Bernd; ASHWEEK, Neil J.; HARRIOTT, Nicole; US2013/143892; (2013); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Sources of common compounds: 7170-01-6

The synthetic route of 7170-01-6 has been constantly updated, and we look forward to future research findings.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Methyl-1H-1,2,4-triazole

EXAMPLE 102 [2-Chloro-4-(3-methyl-1,2,4-triazol-1-yl)-phenyl](5H,11H-pyrrolo[2,1-c]-[1,4]benzodiazepin-10-yl)-methanone To a suspension of 60% sodium hydride in oil (0.3 g) in dimethylformamide (50 ml) was added dropwise 3-methyl-1,2,4-triazole (0.45 g).. After hydrogen gas evolution ceased, 2-chloro-4-fluorophenyl-(5H,11H-pyrrolo[2,1-c][1,4]benzodiazepine-10-yl)-methanone (1.70 g) was added and the reaction mixture was heated in a sand bath at 110 C for 18 hours.. The mixture was poured onto ice, diluted with brine, and extracted with dichloromethane.. The combined extracts were dried over anhydrous sodium sulfate and filtered through a short column of anhydrous sodium magnesium silicate.. The solution was concentrated in vacuo and the residue was triturated with diethyl ether to give 1.25 g of the title compound as colorless crystals, m.p. 191-193 C, MS m/z: 404.1 (M+H)+.

The synthetic route of 7170-01-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wyeth; EP1000062; (2004); B1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

The important role of 7170-01-6

According to the analysis of related databases, 7170-01-6, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 7170-01-6 as follows. Product Details of 7170-01-6

Procedure: A 500 mL round bottom flask was loaded with 4-methoxy-7-chloro-6-azaindole precursor 2e (9.1 g, 50 mmol; dried in vacuo), potassium carbonate (13.8 g, 100 mmol, 2 eq.), copper powder (6.35 g, 100 mmol, 2 eq.), and 3-methyl-1,2,4-triazole (83 g, 1.0 mol, 20 eq.). The solid mixture was heated to melt at 170-175 C. (external oil bath temperature) under gentle stream of anhydrous nitrogen for 12 h, by which time HPLC analysis indicates the amount of the peak for the starting material becomes 5-30% and the desired product peak becomes about 45% with isomeric by-product peak becomes 15%. As the reaction mixture cools, MeOH (150 mL) was added slowly to the stirred warm mixture. Upon cooling, the insoluble material (copper powder) was filtered through a Celite pad, and rinsed with methanol. The filtrate was concentrated in vacuo to a thick paste which was diluted with water (1 L) and extracted with EtOAc (3¡Á150 mL). The EtOAc extracts were dried (MgSO4), filtered and concentrated to obtain about 8 g of crude residue which was crystallized by dissolving in hot CH3CN (50 mL), followed by diluting with water (100 mL) and cooling at 0 C. to collect 1.45 g (12.7%) of the title compound as white solid. The filtrate was purified by C-18 reverse phase silica gel (YMC ODS-A 75 mum) eluted with 15-30% CH3CN/H2O. Appropriate fractions were combined and the aqueous solution after removing CH3CN by rotary evaporator was lyophilized to give additional 1.15 g of the title compound 3-81. The crude aqueous layer was further extracted with EtOAc several times. The ethyl acetate extracts were dried (MgSO4), filtered, concentrated, and crystallized from MeOH to give additional 200 mg of the title compound 3-81. The total yield: 2.8 g (12.2 mmol, Y. 24.5%); MS m/z 230 (MH), HRMS (ESI) m/z calcd for C11H12N5O (M+H), 230.1042, found 230.1038 (Delta-1.7 ppm); 1H NMR (CDCl3) delta ppm 2.54 (3H, s, CH3), 4.05 (3H, s, OCH3), 6.73 (1H, s, H-3), 7.40 (1H, s, H-2), 7.56 (1H, s, H-5), 9.15 (1H, s, triazole-H-5); 13C NMR (CDCl3, 125.7 MHz) delta ppm 14.2 (triazole-Me), 56.3 (OMe), 100.5 (C-3), 116.9 (C-5), 123.5, 127.2, 127.5 (C-2), 129.5 (C-7), 141.2 (C-5′), 149.5 (C-4), 161.8 (C-3′); Anal. Calcd for C11H11N5O:C 57.63, H 4.83, N 30.55, found C 57.37, H 4.64, N 30.68. [1514] The structure was confirmed by a single X-ray crystallographic analysis using crystals obtained from C-18 column fractions. A portion of C-18 column fractions containing a mixture of the desired 3-methyl-1,2,4-triazolyl analog 3-81 and isomeric 5-methy-1,2,4-triazolyl analog 4-81 was further purified by C-18 reverse phase column eluting with 8-10% CH3CN/H2O. Appropriate fractions were extracted with CH2Cl2, and slow evaporation of the solvent gave crystalline material of the isomeric 7-(5-methy-1,1,2,4-triazolyl)-4-methoxy-6-azaindole (4-81): MS m/z 230 (MH), 1H NMR (CDCl3) delta ppm 3.05 (3H, s, CH3), 4.07 (3H, s, OCH3), 6.74 (1H, q, J=2.4, H-2), 7.37 (1H, t, J=2.4, H-3), 7.65 (1H, s, H-5), 8.07 (1H, s, triazole-H-3). The structure was confirmed by a single X-ray crystallographic analysis.

According to the analysis of related databases, 7170-01-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Wang, Tao; Zhang, Zhongxing; Meanwell, Nicholas A.; Kadow, John F.; Yin, Zhiwei; Xue, Qiufen May; Regueiro-Ren, Alicia; Matiskella, John D.; Ueda, Yasutsugu; US2004/110785; (2004); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Some scientific research about 7170-01-6

The synthetic route of 7170-01-6 has been constantly updated, and we look forward to future research findings.

Electric Literature of 7170-01-6, A common heterocyclic compound, 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, molecular formula is C3H5N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a solution of 2-chloro-4-fluorobenzaldehyde (95 mmol, 15 g) and 3-methyl-lH-l,2,4-triazole (114 mmol, 9.4 g) in CH3CN (300 mL) was added K2C03 (142 mmol, 20 g) and stirred at 60 C. After 24 h, the reaction mixture was added water and extracted with EtOAc. The organic extracts washed with saturated aq. NaCl, dried over Na2S04, filtered and concentrated in vacuo. The crude was purified by column chromatography (heptane: EtOAc = 20:80-10:90) to give the title compound. MS (ESI) m/z = 222, 224 (M+H) 1H NMR (300 MHz, CDC13) delta (ppm): 10.45 (1H, s), 8.55 (1H, s), 8.06 (1H, d, J= 8.6 Hz), 7.87 (1H, d, J= 2.1 Hz), 7.68 (1H, dd, J= 8.6, 2.1 Hz), 2.51 (3H, s).

The synthetic route of 7170-01-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; MOCHIDA PHARMACEUTICAL CO., LTD.; SAKURADA, Isao; HIRABAYASHI, Tomokazu; MAEDA, Yoshitaka; NAGASUE, Hiroshi; MIZUNO, Takashi; XU, Jiayi; ZHANG, Ting; SMITH, Cameron; PARKER, Dann; WO2015/160634; (2015); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Continuously updated synthesis method about 7170-01-6

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, A new synthetic method of this compound is introduced below., Recommanded Product: 7170-01-6

EXAMPLE 103 [4-(3-Methyl-1,2,4-triazol-1yl)-2-trifluoromethyl-phenyl](5H,11H-pyrrolo[2,1-c][1,4]benzodiazepin-10-yl)-methanone To a suspension of 60% sodium hydride in oil (0.3 g) in dimethylformamide (50 ml) was added dropwise 3-methyl-1,2,4-triazole (0.45 g). After hydrogen gas evolution ceased, 4-fluoro-2-trifluoromethyl-phenyl-(5H,11H-pyrrolo[2,1-c][1,4]-benzodiazepine-10-yl)-methanone (1.76 g) was added and the reaction mixture was heated in a sand bath at 110 C. for 18 hours. The mixture was poured onto ice, diluted with brine, and extracted with dichloromethane. The combined extracts were dried over anhydrous sodium sulfate and filtered through a short column of anhydrous sodium magnesium silicate. The solution was concentrated in vacuo and the residue was triturated with diethyl ether to give 0.81 g of the title compound as colorless crystals, m.p. 148-150 C., MS m/z: 438.2 (M+H)+, 875.8 (2M+H)+.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Wyeth; US6511974; (2003); B1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Simple exploration of 7170-01-6

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Methyl-1H-1,2,4-triazole, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, belongs to Triazoles compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 7170-01-6, SDS of cas: 7170-01-6

To a solution of l-chloro-2-(4-methoxybenzyloxy)-4-nitrobenzene (15 g, 51.1 mmol) in DMSO (45 mL) was added potassium hydroxide (4.3 g, 77 mmol) followed by methyl triazole (6.39 g, 77 mmol) at room temperature. The reaction mixture was heated at 95 C for 18 h. The reaction mixture was poured onto crushed ice (1.5 Kg) and extracted with ethyl acetate (3 x 250 mL). It was then washed with brine (3 x 250 mL) and dried over sodium sulphate. The solvent was removed under reduced pressure and the residue was dissolved in dichloromethane (25 mL) and absorbed onto silica (25 g). The resultant slurry of the compound on silica was subjected to flash chromatography using a Teledyne Isco instrument (120 g RediSep silica column, with 50% ethyl acetate in pet-ether) to get Intermediate J(2) (6 g, 34.5%) as a yellow solid and Intermediate J(3) (4.5 g, 24.9%) as a dark brown solid.Analytical data of J(2): LC-MS (M+H)+ = 341.2. IH NMR (400 MHz, CDC13) delta ppm 8.83 (IH, s), 8.13 (IH, d, J=8.8 Hz), 8.06 (IH, s), 8.09 (IH, d, J= 8.8 Hz), 7.35 (2H, d, J=8.4 Hz), 6.94 (2H, d, J= 6.4 Hz), 5.29 (2H, s), 3.83 (3H, s), 2.47 (3H, s).Analytical data of J(3): LC-MS (M+H)+ = 341.2. IH NMR (400 MHz, CDC13) delta ppm 8.03-7.96 (3H, m), 7.57 (IH, d, J= 8.8 Hz), 7.20 (2H, d, J=8.4 Hz), 6.89 (2H, d, J=8.8 Hz), 5.13 (2H, s), 3.80 (3H, s), 2.32 (3H, s).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Methyl-1H-1,2,4-triazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; BOY, Kenneth M.; GUERNON, Jason M.; MACOR, John E.; THOMPSON III, Lorin A.; WU, Yong-Jin; ZHANG, Yunhui; WO2012/9309; (2012); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Share a compound : 7170-01-6

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Methyl-1H-1,2,4-triazole, other downstream synthetic routes, hurry up and to see.

Application of 7170-01-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole belongs to Triazoles compound, it is a common compound, a new synthetic route is introduced below.

A solution of 2,4-difluorobenzonitrile (7.07 g, 50.8 mmol) and 3-methyl-lH- 1,2,4-triazole (4.22 g, 50.8 mmol) in N,N-dimethylformamide (45 ml) was treated with powdered anhydrous potassium carbonate (10 g) and the resulting mixture stirred at 22 C for 18h. The solid was then filtered and the filtrate concentrated in vacuo. The residue was diluted with ethyl acetate, washed with water and brine, then dried over anhydrous magnesium sulfate and concentrated. The resulting mixture was purified by a combination of chromatography on silica gel (elution gradient of ethyl acetate in hexane) and reversed phase silica gel to yield intermediates 81-84.Intermediate 814Fluoro-2-(3-methyl-lH-l,2,4-triazol-l-yl)benzonitrile. White crystals (ethyl acetate-hexane); mp 117-118 0C. 1HNMR 400 MHz (CDCl3) delta ppm: 2.54 (3H, s, CH3), 7.24 (IH5 m, CH), 7.62 (IH, dd, J = 2.5 Hz and J = 9.1 Hz, CH), 7.84 (IH, dd, J = 5.6 Hz and J = 8.6 Hz, CH), 8.82 (IH, s, CH). Anal. Calcd for C10H7FN4: C 59.40, H 3.49, N 27.71; Found: C 59.25, H 3.32, N 27.81. Intermediate 824-Fluoro-2-(5-methyI-lH-l,2,4-fiiazoI-l-yl)benzonifrile. White crystals(ethyl acetate-hexane); mp 120-121 C. 1HNMR 400 MHz (CDCl3) delta ppm: 2.56 (3H, s, CH3), 7.30 (IH, dd, J = 2.5 Hz and J = 8.1 Hz, CH), 7.39 (IH, m, CH), 7.91 (IH, dd, J = 5.5 Hz and J = 8.6 Hz, CH), 8.06 (IH, s, CH). Anal. Calcd for C10H7FN4: C 59.40, H 3.49, N 27.71; Found: C 59.35, H 3.70, N 27.77.Intermediate 832-Fluoro-4-(3-methyl-lH-l,2,4-triazol~l-yl)benzonitrile. White crystals(ethyl acetate-hexane); mp 133-134 C. 1HNMR 400 MHz (CDCl3) deltappm: 2.52 (3H, s, CH3), 7.61 (IH, dd, J = 2 Hz and J = 9.1 Hz, CH), 7.67 (IH, dd, J = 2 Hz and J = 9.6 Hz, CH), 7.79 (IH, dd, J = 6.5 Hz and J = 8.6 Hz, CH), 8.56 (IH, s, CH). Anal. Calcd for C10H7FN4: C 59.40, H 3.49, N 27.71; Found: C 59.42, H 3.24, N 28.41.Intermediate 84 2-Fluoro-4-(5-methyl-lH-l,2,4-triazol-l-yl)ben?onitrile. White crystals (ethyl acetate-hexane); mp 89-90 C, 1HNMR 400 MHz (CDCl3) delta ppm: 2.69 (3H, s, CH3), 7.49-7.55 (2H, m, 2 x CH), 7.83 (IH, dd, J = 6.8 Hz and J = 8.8 Hz, CH), 8.00 (IH, s, CH). Anal. Calcd for Ci0H7FN4: C 59.40, H 3.49, N 27.71; Found: C 59.17, H 3.22, N 28.01.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Methyl-1H-1,2,4-triazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2007/64316; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Brief introduction of 7170-01-6

The synthetic route of 3-Methyl-1H-1,2,4-triazole has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Product Details of 7170-01-6

Intermediate 64 and 654-Fluoro-2-(3-methyl-lH-l,2,4-triazol-l-yl)benzonitrile and 4-fluoro-2-(5- methyl-lH-l,2,4-triazol-l-yl)benzonitrile. A solution of 2,4-difluorobenzonitrile (7.07 g, 50.8 mmol) and 3-methyl-lH-l,2,4-triazole (4.22 g, 50.8 mmol) in N5N- dimethylformamide (45 ml) was treated with powdered anhydrous potassium carbonate (10 g) and the resulting mixture was stirred at 22 0C for 18h. The solid was then filtered and the filtrate was concentrated in vacuo. The residue was diluted with ethyl acetate, washed with water and brine, dried over anhydrous magnesium sulfate and concentrated. The mixture containing the 2 and 4-triazolyl-benzonitriles was purified by a combination of chromatography on silica gel ( elution gradient of ethyl acetate in hexane) and on reversed phase silica gel to give 1.86 g (18 % yield) of Intermediate 64 and 0.526 g (5 % yield) of Intermediate 65.4-Fluoro-2-(3-methyl-lH-l ,2,4-triazol-l -yl)benzonitrile. white crystals (ethyl acetate – hexane) ; mp 117 – 1180C. 1HNMR 400 MHz (CDCl3) delta (ppm) : 2.54 (3H5 S5 CH3), 7.24 (IH5 m5 CH)5 7.62 (IH5 dd5 J = 2.5 Hz and J = 9.1 Hz5 CH)5 7.84 (IH5 dd, J = 5.6 Hz and J = 8.6 Hz5 CH)5 8.82 (IH, s, CH). Anal. Calcd for Ci0H7FN4: C 59.40, H 3.49, N 27.71; Found: C 59.25, H 3.32, N 27.81.4-fluoro-2-(5-methyl-lH-l,2,4-triazol-l-yl)benzonitrile. white crystals (ethyl acetate -hexane); mp 120 – 121 0C. 1HNMR 400 MHz (CDCl3) delta (ppm) : 2.56 (3H, s, CH3), 7.30 (IH, dd, J = 2.5 Hz and J = 8.1 Hz5 CH)5 7.39 (IH5 m, CH), 7.91 (IH, dd5 J = 5.5 Hz and J = 8.6 Hz, CH), 8.06 (IH5 s, CH). Anal. Calcd for Ci0H7FN4: C 59.40, H 3.49, N 27.71; Found: C 59.35, H 3.70, N 27.77.

The synthetic route of 3-Methyl-1H-1,2,4-triazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2007/58646; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Analyzing the synthesis route of 7170-01-6

The synthetic route of 3-Methyl-1H-1,2,4-triazole has been constantly updated, and we look forward to future research findings.

Reference of 7170-01-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole belongs to Triazoles compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 3-methyl-lH-l,2,4-triazole (15.0 g, 181 mmol), 1,2- difluoro-4-nitrobenzene (28.7 g, 181 mmol), and sodium bicarbonate (15.2 g, 181 mmol) in DMSO (100 mL) was heated at 80 0C for 48 h . The reaction mixture was allowed to cool to rt and was poured into water (800 mL). The aqueous mixture was extracted with EtOAc (3 x 200 mL). The combined organic extracts were sequentially washed with water (500 mL) and brine solution (100 mL). The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. The crude reaction mixture was purified using silica gel chromatography (30-80% EtOAc/hexane, linear gradient) to afford two regioisomeric products. Pure fractions of the less polar regioisomer were combined and concentrated to afford l-(2-fluoro- 4-nitrophenyI)-3-methyl-lH-l,2>;4-triazole (7.2 g, 30.8 mmol, 17 % yield) as an off- white solid. Pure fractions of the more polar regioisomer were combined and concentrated to afford l-(2~fluoro-4-nitrophenyl)-5-methyl-lH-l52,4-triazoIe (6.23 g, 28.0 mmol, 15 % yield) as an off-white solid. Data for l-(2-fluoro-4-nitrophenyl)-5-methyHH-l,2,4-triazole: LC-MS(M+H)+ = 223.1. 1HNMR (500 MHz, chloroform-*/) delta ppm 8.18 – 8.24 (m, 2 H) 8.04 (s, 1 H) 7.69 – 7.78 (m, 1 H) 2.47-2.53 (m, 3 H).Data for 1 -(2-fluoro-4-nitrophenyl)-3 -methyl- 1 H- 1 ,2,4-triazole: LC-MS (M+H)+ = 223.1. 1H NMR (500 MHz, chloroform-tO delta ppm 8.73 (d, J-2.7 Hz5I H), 8.15 – 8.26 (m, 3 H), 2.53 (s, 3 H).

The synthetic route of 3-Methyl-1H-1,2,4-triazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; MARCIN, Lawrence, R.; THOMPSON, Lorin, A., III; BOY, Kenneth, M.; GUERNON, Jason, M.; HIGGINS, Mendi, A.; SHI, Jianliang; WU, Yong-Jin; ZHANG, Yunhui; MACOR, John, E.; WO2010/83141; (2010); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Sources of common compounds: 7170-01-6

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 7170-01-6, its application will become more common.

Some common heterocyclic compound, 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, molecular formula is C3H5N3, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. category: Triazoles

Synthesis of 1-fluoro-2-methoxy-4-nitrobenzene (1023) To a stirred solution of 1-fluoro-2-methoxy-4-nitrobenzene (2.5 g, 14.60 mmol) in DMF (25 mL) under an argon atmosphere were added potassium carbonate (4 g, 29.20 mmol) and 3-methyl-1H-1,2,4-triazole (1.2 g, 14.60 mmol) at room temperature. The reaction mixture was stirred at 85 C. for 16 h in a sealed tube. After consumption of the starting material (monitored by TLC), the reaction mixture was diluted with water (100 mL) and extracted with EtOAc (2¡Á50 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was purified by column chromatography using 15-25% EtOAc:hexane to afford 1-fluoro-2-methoxy-4-nitrobenzene (1.2 g, 35%) as an off-white solid. 1H-NMR (CDCl3, 400 MHz): delta 8.87 (s, 1H), 8.10 (d, 1H), 8.00-7.97 (m, 2H), 4.10 (s, 3H), 2.50 (s, 3H); LCMS: 234.9 (M+1); (column; Ascentis Express C-18 (50¡Á3.0 mm, 2.7 mum); RT 2.02 min. 0.025% Aq TFA+5% ACN: ACN+5% 0.025% Aq TFA; 1.2 mL/min); TLC: 30% EtOAc:hexane (Rf: 0.2).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 7170-01-6, its application will become more common.

Reference:
Patent; FORUM Pharmaceuticals Inc.; Burnett, Duane A.; Bursavich, Matthew Gregory; McRiner, Andrew J.; (484 pag.)US2017/44182; (2017); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics