تفاعل #452422

معادلة التفاعل

5-chloro-2-pentanone

dimethylamine hydrochloride

potassium carbonate

→

desired product

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

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 2 hours
2. 2
   درجة الحرارةThe reaction mixture was then cooled to room temperature
3. 3
   أخرىpartitioned between water and dichloromethane
4. 4
   أخرىThe phases were separated
5. 5
   استخلاصthe aqueous phase again extracted with dichloromethane
6. 6
   تجفيفdried over sodium sulfate
7. 7
   تركيزconcentrated under reduced pressure
8. 8
   غسيلeluting with dichloromethane containing 10% methanol and 1% ammonium hydroxide
9. 9
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

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.

المصدر