HRID1242354
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
- 100 °C
PROCEDURE
实验过程
A mixture of 25 g (90 mmol) of the above prepared [2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-yl]-acetonitrile, 20 g of sodium hydroxide (500 mmol), 60 ml of water, and 250 ml of propanol was stirred vigorously at 100° C. Hydrolysis was complete after 2 hours. The reaction mixture was then evaporated to dryness and the residue was redissolved in 70 ml of water; 60 ml of cold 8 N aqueous HCl was then added and the acid extracted with three portions of 250 ml of ethyl acetate; the combined organic phases were washed with water and brine, dried over sodium sulfate, and evaporated to dryness. Thereby, 25.1 g of the title product was obtained as pale yellow solid.
WORKUP
后处理
- additionA mixture of 25 g (90 mmol) of the
- customHydrolysis
- customThe reaction mixture was then evaporated to dryness
- dissolutionthe residue was redissolved in 70 ml of water
- addition60 ml of cold 8 N aqueous HCl was then added
- extractionthe acid extracted with three portions of 250 ml of ethyl acetate
- washthe combined organic phases were washed with water and brine
- dry with materialdried over sodium sulfate
- customevaporated to dryness