반응 #318032

반응 방정식

3-(4-bromo-1-methyl-1H-pyrazol-3-yl)aniline

sodium carbonate

→

title compound

수율 72.8%

3-(1-Methyl-1H-pyrazol-3-yl)aniline

수율 72.8%

용매

ethanol

ethanol

반응 조건

후처리

1. 1
   여과The mixture was filtered through ‘hyflo’
2. 2
   여과filter aid
3. 3
   세척the filter pad washed with ethanol (50 ml)
4. 4
   기타The combined filtrate was evaporated in vacuo
5. 5
   기타to give a brown gum
6. 6
   추출extracted with ethyl acetate (2×100 ml)
7. 7
   건조the organic layer was dried over magnesium sulphate
8. 8
   기타the solvent removed in vacuo
9. 9
   기타Purification by chromatography on silica gel
10. 10
    세척eluting with diethyl ether

실험 절차

A solution of 3-(4-bromo-1-methyl-1H-pyrazol-3-yl)aniline (1.0 g) (available from Maybridge) in ethanol (20 ml) was added to a pre-hydrogenated suspension of 5% palladium on charcoal (0.5 g) in ethanol (40 ml). The resulting suspension was stirred under an atmosphere of hydrogen for 3 h. The mixture was filtered through ‘hyflo’ filter aid and the filter pad washed with ethanol (50 ml). The combined filtrate was evaporated in vacuo to give a brown gum. This gum was treated with 2M sodium carbonate solution (100 ml) and extracted with ethyl acetate (2×100 ml); the organic layer was dried over magnesium sulphate and the solvent removed in vacuo. Purification by chromatography on silica gel, eluting with diethyl ether, gave the title compound as a white crystalline solid (0.5 g).

출처