Реакция #452422

Уравнение реакции

5-chloro-2-pentanone

dimethylamine hydrochloride

potassium carbonate

→

desired product

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

Растворители

acetonitrile

Условия реакции

Обработка

1. 1
   Температураat reflux for 2 hours
2. 2
   ТемператураThe reaction mixture was then cooled to room temperature
3. 3
   Другоеpartitioned between water and dichloromethane
4. 4
   ДругоеThe phases were separated
5. 5
   Экстракцияthe aqueous phase again extracted with dichloromethane
6. 6
   Сушкаdried over sodium sulfate
7. 7
   Концентрированиеconcentrated under reduced pressure
8. 8
   Промывкаeluting with dichloromethane containing 10% methanol and 1% ammonium hydroxide
9. 9
   Концентрированиеconcentrated under reduced pressure

Методика

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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