HRID1994434

反应详情

EQUATION

反应方程式

HRID 1994434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

0.08 g (0.168 mmol) of methyl 2-benzyloxycarbonylamino-3-(2,4-dichlorobenzenesulfonylamino)-2-methylpropionate and 0.093 g (0.674 mmol) of potassium carbonate are stirred in a mixture of 4.5 ml of MeOH and 0.5 ml of water for 90 min. Then 3 ml of saturated NaHCO3 solution are added, and the mixture is stirred at 60° C. for 2 h. 0.5 ml of water is added, followed by 4N HCl (aq) until a pH of 2 is reached. The solution is extracted 3 times with 10 ml of EtOAc each time, the combined organic phases are dried over MgSO4, and the solvent is removed in vacuo. 68 mg of the desired product are obtained. MW=460 (calculated, monoisotopic), measured value: (M+H)+461.

WORKUP

后处理

  1. extractionThe solution is extracted 3 times with 10 ml of EtOAc each time
  2. dry with materialthe combined organic phases are dried over MgSO4
  3. customthe solvent is removed in vacuo