HRID20320

反应详情

EQUATION

反应方程式

HRID 20320 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 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (100 mg) and Montmorillonite KSF clay (100 mg) in acetonylacetone (1 ml) was heated at 120° C. (50 W) for 15 minutes in a CEM discover microwave synthesiser. The reaction mixture was diluted with 5% methanol/dichloromethane, filtered and evaporated. The crude product was purified by flash column chromatography eluting with 1:2 ethyl acetate/hexane, and the product containing fractions were combined and evaporated to give 65 mg of the target molecule as a pale brown solid. (LC/MS: Rt 3.75 [M+H]+ 299).

WORKUP

后处理

  1. filtrationfiltered
  2. customevaporated
  3. customThe crude product was purified by flash column chromatography
  4. washeluting with 1:2 ethyl acetate/hexane
  5. additionthe product containing fractions
  6. customevaporated
  7. customto give 65 mg of the target molecule as a pale brown solid