反应 #80266

ord-02cacc73113c408c9974ae03a4320444

反应方程式

CN(CCOC(=O)Oc1ccccc1)CCOC(=O)Oc1ccccc1
N,N-bis[2-((phenoxycarbonyl)oxy)ethyl]-N-methylamine
CC#N
acetonitrile
COS(=O)(=O)OC
dimethylsulfate
COS(=O)(=O)[O-].C[N+](C)(CCOC(=O)Oc1ccccc1)CCOC(=O)Oc1ccccc1
4
COS(=O)(=O)[O-].C[N+](C)(CCOC(=O)Oc1ccccc1)CCOC(=O)Oc1ccccc1
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. 1
    其他To a 1000 ml three-necked round-bottomed flask fitted with a reflux condenser, magnetic stirrer
  2. 2
    workup.ADDITIONinternal thermometer, addition funnel, and argon inlet
  3. 3
    workup.ADDITIONAfter addition
  4. 4
    温度the mixture is heated
  5. 5
    温度to reflux for 2 h
  6. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05616546uspto-grants-1997_04