反応 #43531

反応方程式

ethyl acetate

acrylamide

triethylamine

acetyl chloride

→

desired compound

収率 4.0%

N-acetyl methacrylamide

収率 4.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONAfter the termination of the dropwise addition
2. 2
   その他Triethylamine hydrochloride thus precipitated
3. 3
   ろ過was then filtered off
4. 4
   workup.DISTILLATIONThe filtrate was then subjected to distillation under reduced pressure
5. 5
   その他to remove the solvent
6. 6
   その他The residue thus obtained

実験手順

23.7 g of acrylamide and 60 ml of triethylamine were dissolved in 100 ml of dichloromethane in a flask. To the solution was then added dropwise 27.6 g of acetyl chloride at a temperature of −30° C. After the termination of the dropwise addition, the mixture was then stirred at a temperature of 0° C. for 10 hours. Triethylamine hydrochloride thus precipitated was then filtered off. The filtrate was then subjected to distillation under reduced pressure to remove the solvent therefrom. The residue thus obtained was then subjected to column chromatography with ethyl acetate as a developing solvent and silica gel as a filler to obtain 1.5 g of the desired compound (yield: 4%).

出典