反応 #487538

反応方程式

water

N,O-dimethylhydroxyamine hydrochloride

Decanoic acid

→

N-methoxy-N-methyldecanamide

収率 97.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONwas then added to the solution
2. 2
   workup.STIRRINGthe obtained mixture was further stirred for 3 hours
3. 3
   抽出the reaction solution was extracted with dichloromethane two times
4. 4
   workup.ADDITIONAnhydrous magnesium sulfate was added to the organic layer
5. 5
   その他to dry it
6. 6
   ろ過the resultant was filtrated
7. 7
   濃縮was then concentrated
8. 8
   その他The obtained residue was purified

実験手順

Decanoic acid (4 g, 23.2 mmol) was dissolved in an anhydrous dichloromethane solution (80 mL), and 1,1-carbonyldiimidazole (4.5 g, 27.9 mmol) was then added to the solution, followed by stirring for 1.5 hours. Subsequently, N,O-dimethylhydroxyamine hydrochloride (2.7 g, 27.9 mmol) was added to the reaction solution, and the obtained mixture was further stirred for 3 hours. After addition of distilled water, the reaction solution was extracted with dichloromethane two times. Anhydrous magnesium sulfate was added to the organic layer to dry it, and the resultant was filtrated and was then concentrated. The obtained residue was purified using column chromatography (hexane:ethyl acetate=8:1), so as to obtain N-methoxy-N-methyldecanamide (4.8 g, 97%) as an amide body in the form of a colorless transparent liquid.

出典