反応 #531835

ord-8ac65ce9a4be4d18aa7ec3d430ae4bb8

反応方程式

CCCCNC
N-butyl-N-methylamine
C(=NC1CCCCC1)=NC1CCCCC1
dicyclohexylcarbodiimide
C(=NC1CCCCC1)=NC1CCCCC1
dicyclohexylcarbodiimide
CCCCN(C)C(=NC1CCCCC1)NC1CCCCC1
guanidine
収率 99.7%
CCCCN(C)C(=NC1CCCCC1)NC1CCCCC1
1-Butyl-2,3-dicyclohexyl-1-methylguanidine
収率 99.7%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度is heated
  2. 2
    温度at reflux for 3 hours
  3. 3
    濃縮is concentrated at 60° C. under 1 mbar for 2 hours
  4. 4
    その他to give 29.9 g of a colorless and virtually odorless liquid of medium viscosity

実験手順

A mixture of 17.78 g of N-butyl-N-methylamine (0.204 mol) and 21.05 g of dicyclohexylcarbodiimide (0.102 mol) is heated at reflux for 3 hours. GC analysis then shows a conversion of more than 99.5% of the dicyclohexylcarbodiimide. The final mixture, which is colorless, is concentrated at 60° C. under 1 mbar for 2 hours, to give 29.9 g of a colorless and virtually odorless liquid of medium viscosity, corresponding to the expected guanidine (99.7% yield).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08475873B2uspto-grants-2013_07