反应 #80266
ord-02cacc73113c408c9974ae03a4320444
反应方程式
N,N-bis[2-((phenoxycarbonyl)oxy)ethyl]-N-methylamine
acetonitrile
dimethylsulfate
→
4
N,N-Bis[2-((phenoxycarbonyl)oxy)ethyl]-N,N-dimethylammonium Methylsulfate
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他To a 1000 ml three-necked round-bottomed flask fitted with a reflux condenser, magnetic stirrer
- 2workup.ADDITIONinternal thermometer, addition funnel, and argon inlet
- 3workup.ADDITIONAfter addition
- 4温度the mixture is heated
- 5温度to reflux for 2 h
- 6其他The product precipitates from the mixture after approximately 15 min
实验过程
To a 1000 ml three-necked round-bottomed flask fitted with a reflux condenser, magnetic stirrer, internal thermometer, addition funnel, and argon inlet are added N,N-bis[2-((phenoxycarbonyl)oxy)ethyl]-N-methylamine (100.00 g, 0.278 mol), acetonitrile (270 ml), and dimethylsulfate (35.93 g, 0.278 mol) over 10 min. After addition is complete, the mixture is heated to reflux for 2 h. The cooled mixture is treated with ether (500 ml). The product precipitates from the mixture after approximately 15 min to give 4 as a white powder, 126.26 g (93%): mp 85°-87° C.