HRID601045

反应详情

EQUATION

反应方程式

HRID 601045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
220 °C

PROCEDURE

实验过程

A mixture of N-cyano-N′-(4-morpholinopheny)-O-phenylisourea (8.76 g, 27.2 mmol, 4-chloro-6-hydrazino-pyrimidine (4.12 g, 28.5 mmol) and di-iso-propylethylamine (18.9 mL, 109 mmol) in N-methyl-pyrrolidinone (50 mL) was heated in the microwave apparatus at 220° C. for 5 min, cooled, poured into ice-water, stirred 0.5 h and filtered to obtain crude product (9.30 g). Purification by flash chromatography (SiO2) eluted with 2:98 methanol:dichloromethane provided the title compound (3.91 g, 39% yield) as a yellow powder.

WORKUP

后处理

  1. temperaturecooled
  2. filtrationfiltered
  3. customto obtain crude product (9.30 g)
  4. customPurification by flash chromatography (SiO2)
  5. washeluted with 2:98 methanol