HRID429324

反应详情

EQUATION

反应方程式

HRID 429324 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1-(3-cyano-4-methoxyphenyl)-5-[4-(methylthio)phenyl]-2-pyrazoline-3-amine (4.0 g) and manganese(IV) oxide (6.0 g) in toluene (100 ml) was stirred at ambient temperature for 8 hours. The insoluble material was filtered and washed with ethyl acetate. The resulting solution was concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel eluting with a mixture of acetone and dichloromethane (1:1) to give partially purified 1-(3-cyano-4-methoxyphenyl)-5-[4-(methylthio)phenyl]pyrazole-3-amine (1.1 g).

WORKUP

后处理

  1. filtrationThe insoluble material was filtered
  2. washwashed with ethyl acetate
  3. concentrationThe resulting solution was concentrated under reduced pressure
  4. additionThe residue was subjected to column chromatography on silica gel eluting with a mixture of acetone and dichloromethane (1:1)