HRID2190498

反应详情

EQUATION

反应方程式

HRID 2190498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of tert-butyl [3-(3,4-diaminophenoxy)phenyl]carbamate (3.00 g, 9.51 mmol) in tetrahydrofuran (150 mL) was added cyanogen bromide (2.93 g, 27.7 mmol), and the mixture was stirred at room temperature for 3 days. The reaction mixture was diluted with ethyl acetate (300 mL), washed with saturated aqueous sodium hydrogencarbonate solution (100 mL×2) and saturated brine (100 mL), successively, and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the filtrate was concentrated to give the title compound (4.37 g) as a brown solid.

WORKUP

后处理

  1. washwashed with saturated aqueous sodium hydrogencarbonate solution (100 mL×2) and saturated brine (100 mL)
  2. dry with materialsuccessively, and dried over anhydrous magnesium sulfate
  3. filtrationThe insoluble material was filtered off
  4. concentrationthe filtrate was concentrated