HRID1242354

反应详情

EQUATION

反应方程式

HRID 1242354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionA mixture of 25 g (90 mmol) of the
  2. customHydrolysis
  3. customThe reaction mixture was then evaporated to dryness
  4. dissolutionthe residue was redissolved in 70 ml of water
  5. addition60 ml of cold 8 N aqueous HCl was then added
  6. extractionthe acid extracted with three portions of 250 ml of ethyl acetate
  7. washthe combined organic phases were washed with water and brine
  8. dry with materialdried over sodium sulfate
  9. customevaporated to dryness