HRID867078

反应详情

EQUATION

反应方程式

HRID 867078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution made from 13.4 g of dicyclopropylmethylamine in 30 ml tetrahydrofuran is added dropwise to a solution of 13 g of β-chloroetyl isocyanate in 15 ml tetrahydrofuran while maintaining the inner temperature from 0° to +5° C. Then, the reaction mixture is kept at room temperature for 15 hours. Afterwards, the solution is evaporated to dryness and the dry residue, weighing 26.5 g, is used as such for the next step of the synthesis. For analytical purpose, a sample of the raw urea is recrystallised from acetonitrile. The N-(dicyclopropylmethyl) N-(β-chloroethyl) urea occurs as white crystals melting at 103°-104° C. with decomposition.

WORKUP

后处理

  1. temperaturewhile maintaining the inner temperature from 0° to +5° C
  2. customAfterwards, the solution is evaporated to dryness
  3. customsuch for the next step of the synthesis
  4. customFor analytical purpose, a sample of the raw urea is recrystallised from acetonitrile