反应详情

4-Chloro-2-fluoro-5-isopropoxyphenylhydrazine (1.8 g), 2-acetylcyclohexanone (1.0 g) and a catalytic amount of acetic acid were dissolved in xylene (5 ml). The resultant mixture was heated under reflux for 8 hours while removing water. After cooling, the reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography to give 0.9 g of 3-methyl-2-(4-chloro-2-fluoro-5-isopropoxyphenyl)-4,5,6,7-tetrahydro-2H-indazole (Compound No. 5). nD14.5 1.5607.

1. temperatureunder reflux for 8 hours
2. customwhile removing water
3. temperatureAfter cooling
4. concentrationthe reaction mixture was concentrated under reduced pressure
5. customthe residue was purified by silica gel column chromatography