HRID1690537

反应详情

EQUATION

反应方程式

HRID 1690537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Copper (I) cyanide (9.76 g, 109 mmol) was added to a solution of (4-chloro-phenyl)-(4,5-difluoro-2-iodo-phenyl)-diazene (5.89 g, 16 mmol) in 1-propanol (95 ml) under an argon atmosphere. The reaction mixture was heated under reflux conditions for 14 h and diluted with CH2Cl2/heptane 1/1 (70 ml). The suspension was filtered and the filtrate was evaporated to dryness to give the title compound (3.3 g, 12 mmol; 77%) as brown solid which was used in the next step without further purification. MS: m/e=278.0 [M+H+].

WORKUP

后处理

  1. temperatureThe reaction mixture was heated under reflux conditions for 14 h
  2. filtrationThe suspension was filtered
  3. customthe filtrate was evaporated to dryness