HRID252240

反应详情

EQUATION

反应方程式

HRID 252240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

4-Bromo-5-chloro-thiophene-2-sulfonyl chloride (0.44 g, 1.50 mmol) and pyridine (0.27 ml, 3.40 mmol) were added to a stirred suspension of sodium cyanate (0.14 g, 2.20 mmol) in dry acetonitrile (1 ml) and the mixture stirred at room temperature for 4 hours. 5-Bromo-thiazol-2-ylamine hydrobromide (0.26 g, 1.00 mmol) was added and the reaction stirred for 30 minutes. Water (2 ml) and acetic acid (3 drops) were added. The resulting precipitate was filtered and the solid washed with water, cold methanol and diethyl ether. The solid was dried under reduced pressure to give 4-bromo-N-[(5-bromo-1,3-thiazol-2-yl)carbamoyl]-5-chlorothiophene-2-sulfonamide, 0.29 g (60%), m/e 477.8 (MH−).

WORKUP

后处理

  1. stirringthe reaction stirred for 30 minutes
  2. filtrationThe resulting precipitate was filtered
  3. washthe solid washed with water, cold methanol and diethyl ether
  4. customThe solid was dried under reduced pressure