反应详情

A mixture of 2-(4-chloro-2-fluoro-5-isopropoxyphenyl)-1,2,4,5,6,7-hexahydro-3H-indazol-3-one (1 g) and phosphorus oxychloride (0.7 g) was heated under reflux heating for 6 hours. After cooling, the reaction mixture was dissolved in chloroform, washed with a 5% sodium hydroxide solution and water, dried and concentrated. The residue was purified by silica gel column chromatography to give 0.3 g of 3-chloro-2-(4-chloro-2-fluoro-5-isopropoxyphenyl)-4,5,6,7-tetrahydro-2H-indazole (Compound No. 2). nD26 1.5530.

1. temperaturewas heated
2. temperatureunder reflux
3. temperatureheating for 6 hours
4. temperatureAfter cooling
5. washwashed with a 5% sodium hydroxide solution and water
6. customdried
7. concentrationconcentrated
8. customThe residue was purified by silica gel column chromatography