HRID495394

反应详情

EQUATION

反应方程式

HRID 495394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydroxide (0.55 g) was dissolved in water (5 ml) and the resulting solution was diluted with ethanol (3 ml). 2-Nitroacetophenone (1.8 g) was added at 20° C., and the solution was stirred for 5 minutes. 3-Chloro-5-(trifluoromethyl)pyridine-2-carboxaldehyde (2.25 g) was added and stirring was continued for 16 hours. The solution was acidified with acetic acid, the organic layer separated, dried over magnesium sulfate, filtered and evaporated to give a brown oil. Silica gel column chromatography, followed by recrystallisation (petrol) afforded the title compound, 88-9° C.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 16 hours
  3. customthe organic layer separated
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customto give a brown oil
  8. customSilica gel column chromatography, followed by recrystallisation (petrol)