According to the analysis of related databases, 41253-21-8, 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 41253-21-8 as follows. Quality Control of Sodium 1,2,4-triazol-1-ide
EXAMPLE 3; Preparation of crude Anustrozole:Tupsilon the title compound of example 2 (50g) in dry DMF (250ml), anhydrous potassium carbonate (26g) and triazole sodium salt (232 g) are added and the mixture stirred at room 25 temperature for 45 min. Worked up the reaction mixture by adding water ( 1500 ml) and extraction with toluene (3 x 300ml). Combined toluene layer is washed with water (1 x300ml), washed toluene layer is dried over anhydous sodium sulphate, fitered and evaporated toluene to obtain crude anastrozole (4Og) having isomeric impurity 0.5%. EXAMPLE 4Preparation of crude Anastrozole:To the title compound of example 2 (500g) in dry DMF (250ml), anhydrous potassium carbonate (26Og) and triazole sodium salt (2320 g) are added and the mixture stirred at room iemperature for 45 min. Worked up the reaction mixture by adding water ( 15000 ml) and extraction with toluene (3 x 3000ml). Combined toluene layer is washed with water ( 1 3000ml), washed toluene layer is dried over anhydrous sodium sulphate, filtered and evaporated toluene to obtain crude anastrozole (45Og) having isomeric impurity 0.5%. EXAMPLE 5 Preparation of crude Anastrozole:To the title compound of example 2 (5Og) in dry DMF (250ml) anhydrous potassium carbonate (26g) and triazole sodium salt (232 g) are added and the mixture stirred at room temperature for 45 min. Worked up the reaction mixture by adding water (750 ml) and extracting with toluene (3 x 300ml). Combined toluene layer is washed with water ( 1 x300ml).The washed toluene layer is dried over anhydrous sodium sulphate, filtered and evaporated toluene to obtain crude anastrozole (42g) having isomeric impurity 4.52%.EXAMPLE 6Preparation of crude Anastrozole: To the title compound of example 2 (5Og) in dry DMF (250ml) anhydrous potassium carbonate (26g) and triazole sodium salt (232 g) are added and the mixture stirred at room temperature for 45 min. Worked up the reaction mixture by adding water (950 ml) and extracting with toluene (3 x 300ml). Combined toluene layer is washed with water ( 1 x30ml).The washed toluene layer is dried over anhydrous sodium sulphate, filtered and evaporated toluene to obtaincrude anastrozole (42g) having isomeric impurity 2.6%.EXAMPLE7Preparation of crude Anastrozole:To the title compound of example 2 (5Og) in dry DMF (250ml) anhydrous potassium carbonate (26g) and triazole sodium salt (232 g) are added and the mixture stirred at room temperature for 45 min. Worked up the reaction mixture by adding water (2500 ml) and extracting with toluene (3 x 300ml). Combined toluene layer is washed with water ( 1 .300ml).The washed toluene layer is dried over anhydrous sodium sulphate, filtered and evaporated toluene to obtain crude anastrozole (42g) having isomeric impurity 3.2%.
According to the analysis of related databases, 41253-21-8, the application of this compound in the production field has become more and more popular.
Reference:
Patent; SHILPA MEDICARE LTD.; WO2007/105231; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics