HRID384743

反应详情

EQUATION

反应方程式

HRID 384743 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 5-bromopyridine-3-sulfonyl chloride (5 g, 17 mmol) in pyridine (10 mL) at 0° C. was added tert-butylamine (3.6 mL, 2 equiv., 34 mmol). The reaction mixture was allowed to warm to room temperature and then heated to 40° C. for 14 h. After this time the crude reaction mixture was again cooled to 0° C. and diluted with dilute HCl (0.05M, 40 mL). The reaction was stirred at 0° C. for 30 min and the resulting precipitate collected by filtration. The solid was washed with water and dried to afford the title compound as a yellow solid (2.12 g, 7.3 mmol, 42%). No further purification was required.

WORKUP

后处理

  1. temperatureheated to 40° C. for 14 h
  2. customAfter this time the crude reaction mixture
  3. temperaturewas again cooled to 0° C.
  4. filtrationthe resulting precipitate collected by filtration
  5. washThe solid was washed with water
  6. customdried