反应 #582576

反应方程式

acetic acid

Sodium hydroxide

2-Nitroacetophenone

ethanol

3-Chloro-5-(trifluoromethyl)pyridine-2-carboxaldehyde

→

title compound

3-[3-Chloro-5-(trifluoromethyl)-2-pyridyl]-1-(2-nitrophenyl)-2-propen-1-one

溶剂

water

反应条件

后处理

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITwas continued for 16 hours
3. 3
   其他the organic layer separated
4. 4
   干燥dried over magnesium sulfate
5. 5
   过滤filtered
6. 6
   其他evaporated
7. 7
   其他to give a brown oil
8. 8
   其他Silica gel column chromatography, followed by recrystallisation (petrol)

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.

来源