HRID51988

反应详情

EQUATION

反应方程式

HRID 51988 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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.

WORKUP

后处理

  1. customTo a 1000 ml three-necked round-bottomed flask fitted with a reflux condenser, magnetic stirrer
  2. additioninternal thermometer, addition funnel, and argon inlet
  3. additionAfter addition
  4. temperaturethe mixture is heated
  5. temperatureto reflux for 2 h
  6. customThe product precipitates from the mixture after approximately 15 min