HRID655975

反应详情

EQUATION

反应方程式

HRID 655975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of triphosgene (89 mg, 0.3 mmol) in THF were added a solution of 2,3-dichlorobenzylamine (100 mg, 0.59 mmol) in THF dropwise and then DIEA (209 μL, 1.2 mmol). The reaction mixture was stirred at rt for 10 min, and 2-(methylamino)ethanol (90 mg, 1.2 mmol) was added. The reaction mixture was stirred at rt for 15 min and purified on RP-HPLC using a mixture of acetonitrile and H2O to give 3-(2,3-dichlorobenzyl)-1-(2-hydroxyethyl)-1-methylurea (70 mg, 44%). LRMS (M+H+) m/z 277.1.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at rt for 15 min
  2. custompurified on RP-HPLC
  3. additiona mixture of acetonitrile and H2O