HRID573281

反应详情

EQUATION

反应方程式

HRID 573281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-chloropyridin-3-amine (2571 mg), K2CO3 (8292 mg), Pd(OAc)2 (180 mg), dppb (682 mg) and CH3CN (25 mL) was stirred at room temperature under Ar atmosphere for 30 min. 6-Chlorohex-1-yne (2565 mg) was added to the mixture, and the mixture was stirred at 80° C. under Ar atmosphere for 24 h. The mixture was filtrated and insoluble material was washed with CH3CN. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (AcOEt/hexane) to give the title compound (600 mg).

WORKUP

后处理

  1. stirringthe mixture was stirred at 80° C. under Ar atmosphere for 24 h
  2. filtrationThe mixture was filtrated
  3. washinsoluble material was washed with CH3CN
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (AcOEt/hexane)