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
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
0.053 g (1.334 mmol) of 2 molar aqueous sodium hydroxide solution was added to 0.114 g (0.334 mmol) of methyl [5-(3-chlorophenyl)-3-methyl-1-pyridin-3-yl-1H-pyrazol-4-yl]acetate (see A1), and the mixture was stirred at 20° C. for 1 h. The methanol formed during the reaction was removed under reduced pressure, and the residue was poured onto a mixture of 10 ml of water and 15 ml of dichloromethane. The aqueous phase was extracted with 15 ml of dichloromethane, acidified with concentrated hydrochloric acid (pH=3) and extracted three times with in each case 15 ml of dichloromethane. Drying of the combined organic phases and removal of the solvent under reduced pressure give 0.050 g (43% of theory) of a light-beige solid of melting point 163° C.
WORKUP
后处理
- customwas removed under reduced pressure
- additionthe residue was poured onto a mixture of 10 ml of water and 15 ml of dichloromethane
- extractionThe aqueous phase was extracted with 15 ml of dichloromethane
- extractionextracted three times with in each case 15 ml of dichloromethane
- customDrying of the combined organic phases and removal of the solvent under reduced pressure
- customgive 0.050 g (43% of theory) of a light-beige solid of melting point 163° C.