HRID601041

反应详情

EQUATION

反应方程式

HRID 601041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of N-cyano-N′-(4-morpholino-phenyl)-O-phenylisourea (0.69 g, 2.14 mmol) and 2-fluoro-4-iodo-phenylhydrazine (0.65 g, 2.57 mmol) in dimetheyl acetamide (4 mL) was heated at 120° C. for 24 h. The reaction is diluted with ethyl acetate, washed with water (3 times) and brine, dried (sodium sulfate) and evaporated. Purification by flash chromatography (SiO2) eluted with 4:96 methanol:dichloromethane, followed by semi-preparative HPLC provided the title compound (0.03 g, 5% yield) as a white lyophilate.

WORKUP

后处理

  1. washwashed with water (3 times) and brine
  2. dry with materialdried (sodium sulfate)
  3. customevaporated
  4. customPurification by flash chromatography (SiO2)
  5. washeluted with 4:96 methanol