反応 #80267

ord-e659b523b6ff4b2e9810a224ef5e9207

反応方程式

CN(CCOC(=O)Oc1ccccc1)CCOC(=O)Oc1ccccc1
N,N-bis[2((phenoxycarbonyl)oxy)ethyl]-N-methylamine
CC#N
acetonitrile
COS(=O)(=O)c1ccc(C)cc1
methyl p-toluenesulfonate
C[N+](C)(CCOC(=O)Oc1ccccc1)CCOC(=O)Oc1ccccc1.Cc1ccc(S(=O)(=O)[O-])cc1
5
C[N+](C)(CCOC(=O)Oc1ccccc1)CCOC(=O)Oc1ccccc1.Cc1ccc(S(=O)(=O)[O-])cc1
N,N-Bis[2-((phenoxycarbonyl)oxy)ethyl]-N,N-dimethylammonium p-Toluene-sulfonate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他To a 250 ml round-bottomed flask fitted with a reflux condenser, magnetic stirrer, and argon inlet
  2. 2
    workup.ADDITIONAfter addition
  3. 3
    温度the mixture is heated
  4. 4
    温度to reflux for 2 h
  5. 5
    その他The product precipitates from the mixture
  6. 6
    その他dried

実験手順

To a 250 ml round-bottomed flask fitted with a reflux condenser, magnetic stirrer, and argon inlet are added N,N-bis[2((phenoxycarbonyl)oxy)ethyl]-N-methylamine (25.00 g, 69.6 mmol), acetonitrile (100 ml), and methyl p-toluenesulfonate (12.95 g, 69.6 mmol). 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 and dried to give 5 as a white powder, 31.14 g (81%): mp 117°-118° C.

出典

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