反应详情

A hydrogen chloride stream is introduced into a solution of 1.0 g. of 21-acetoxy-6α-chloro-11β-hydroxy-16α-methyl-4-pregnene-3,20-dione in 100 ml. of dioxane for 30 minutes at 25° after adding 1.5 g. of dichlorodicyanobenzoquinone. The solution is then heated for 15 hours to 120°. After cooling, the solution is filtered, the filter cake washed with dichloromethane, and the filtrate evaporated under vacuum. The residue of the evaporation is chromatographed on silica gel. With 32-40% acetone-hexane, after recrystallization from acetone-diisopropyl ether, 380 mg. of 21-acetoxy-6-chloro-11β-hydroxy-16α-methyl-1,4,6-pregnatriene-3,20-dione is obtained.

1. temperatureThe solution is then heated for 15 hours to 120°
2. temperatureAfter cooling
3. filtrationthe solution is filtered
4. washthe filter cake washed with dichloromethane
5. customthe filtrate evaporated under vacuum
6. customThe residue of the evaporation
7. customis chromatographed on silica gel
8. customWith 32-40% acetone-hexane, after recrystallization from acetone-diisopropyl ether, 380 mg