HRID2260725

反应详情

EQUATION

反应方程式

HRID 2260725 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1 -tert-butoxycarbonyl-4-methyl-5-benzimidazolylisothiocyanate (7.0 g) in CH2CI2 (600 mL) is added dropwise over 45 minutes to ethylenediamine (8 mL) in solution in CH2Cl2 (200 mL). The mixture is stirred for 3 hours at room temperature. Ether (150 mL) is added to the suspension and the mixture is stirred for 10 minutes at room temperature. The solid is filtered. The filtrate is rotary evaporated, the residue diluted with CH2Cl2 and reprecipitated with ether to afford a second crop. The combined solids are dried overnight in vacuo to afford N-(1-tert-butoxycarbonyl-4-methyl-5-benzimidazolyl)-N'-2-aminoethylthiourea as a white solid.

WORKUP

后处理

  1. stirringthe mixture is stirred for 10 minutes at room temperature
  2. filtrationThe solid is filtered
  3. additionthe residue diluted with CH2Cl2
  4. customreprecipitated with ether
  5. customto afford a second crop
  6. customThe combined solids are dried overnight in vacuo