反应 #452422

反应方程式

5-chloro-2-pentanone

dimethylamine hydrochloride

potassium carbonate

→

desired product

N,N-dimethyl-5-amino-2-pentanone

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度at reflux for 2 hours
2. 2
   温度The reaction mixture was then cooled to room temperature
3. 3
   其他partitioned between water and dichloromethane
4. 4
   其他The phases were separated
5. 5
   萃取the aqueous phase again extracted with dichloromethane
6. 6
   干燥dried over sodium sulfate
7. 7
   浓缩concentrated under reduced pressure
8. 8
   洗涤eluting with dichloromethane containing 10% methanol and 1% ammonium hydroxide
9. 9
   浓缩concentrated under reduced pressure

实验过程

A mixture of 21.77 gm (180.5 mMol) 5-chloro-2-pentanone, 13.40 gm (164.3 mMol) dimethylamine hydrochloride and 50.0 gm (361.8 mMol) potassium carbonate in 150 mL acetonitrile was stirred at room temperature for 2 days and then at reflux for 2 hours. The reaction mixture was then cooled to room temperature and partitioned between water and dichloromethane. The phases were separated and the aqueous phase again extracted with dichloromethane. All organic phases were combined, dried over sodium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography, eluting with dichloromethane containing 10% methanol and 1% ammonium hydroxide. Fractions shown to contain product were combined and concentrated under reduced pressure. The desired product was then isolated by distillation.

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