반응 #219240

반응 방정식

4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide

Montmorillonite KSF

→

4-(2,5-Dimethyl-pyrrol-1-yl)-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide

용매

methanol dichloromethane

acetonylacetone

반응 조건

후처리

1. 1
   여과filtered
2. 2
   기타evaporated
3. 3
   기타The crude product was purified by flash column chromatography
4. 4
   세척eluting with 1:2 ethyl acetate/hexane
5. 5
   workup.ADDITIONthe product containing fractions
6. 6
   기타evaporated
7. 7
   기타to give 65 mg of the target molecule as a pale brown solid

실험 절차

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).

출처