반응 #452422

반응 방정식

5-chloro-2-pentanone

dimethylamine hydrochloride

potassium carbonate

→

desired product

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

용매

acetonitrile

반응 조건

후처리

1. 1
   온도at reflux for 2 hours
2. 2
   온도The reaction mixture was then cooled to room temperature
3. 3
   기타partitioned between water and dichloromethane
4. 4
   기타The phases were separated
5. 5
   추출the aqueous phase again extracted with dichloromethane
6. 6
   건조dried over sodium sulfate
7. 7
   농축concentrated under reduced pressure
8. 8
   세척eluting with dichloromethane containing 10% methanol and 1% ammonium hydroxide
9. 9
   농축concentrated under reduced pressure

실험 절차

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.

출처