反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 5-(4-fluoro-phenyl)-2-methyl-thiazole-4-carboxylic acid methyl ester (15 g) in a mixture of THF (60 mL) and MeOH (20 mL) was added a solution of sodium hydroxide (2.63 g) in water (60 mL). The reaction mixture was stirred at RT for 30 min. The reaction mixture was then concentrated in vacuo, and the residue was dissolved with water (100 mL) and concentrated again in vacuo. The residue was dissolved in water (250 mL), cooled to 0° C. with a ice-bath. Then was added a solution of conc.HCl (37%)(7.72 g) in water (7.72 g) and stirred at 0° C. for 15 min. The resulting precipitate was filtered off, washed with water and dried in high vacuum pump. to give the title compound as a white solid (13.16 g, 93%).
WORKUP
后处理
- concentrationThe reaction mixture was then concentrated in vacuo
- dissolutionthe residue was dissolved with water (100 mL)
- concentrationconcentrated again in vacuo
- dissolutionThe residue was dissolved in water (250 mL)
- temperaturecooled to 0° C. with a ice-bath
- additionThen was added a solution of conc
- stirringHCl (37%)(7.72 g) in water (7.72 g) and stirred at 0° C. for 15 min
- filtrationThe resulting precipitate was filtered off
- washwashed with water
- customdried in high vacuum pump