HRID601053

反应详情

EQUATION

反应方程式

HRID 601053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A mixture of 1-(2-fluoro-4-iodo-phenyl)-N3-(4-morpholino-phenyl)-1H-[1,2,4]triazole-3,5-diamine (0.48 g, 0.99 mmol) and copper (I) cyanide (0.09 g, 0.99 mmol) in HMPA (3 mL) was heated at 55° C. for 2 h, then poured into water (75 mL) and filtered, washing with water. The filter cake was suspended in chloroform (100 mL) and methanol (5 mL), was refluxed for 2 h, cooled, filtered and evaporated. Purification by semi-preparative HPLC provided the title compound (0.04 g, 9% yield) as a pale tan lyophilate.

WORKUP

后处理

  1. filtrationfiltered
  2. washwashing with water
  3. temperaturemethanol (5 mL), was refluxed for 2 h
  4. temperaturecooled
  5. filtrationfiltered
  6. customevaporated
  7. customPurification by semi-preparative HPLC