反应详情

A solution of 10 g of androsta-1,4-diene-3,17-dione in 95 ml of carbon tetrachloride is refluxed with 6.4 g of N-bromosuccinimide and 0.4 g of benzoyl peroxide for seventy five minutes. After filtration of succinimide, the filtrate was cooled in ice until crystallization is complete. The mixture is then filtered and dried so obtaining 9.8 g of crude 6-bromoandrosta-1,4-diene-3,17-dione satisfactory for the next step. The analytical sample is crystallized from diethyl ether/n-hexane, m.p. 188°-190° C., [α]D20° +116, U.V. (95% EtOH) λmax=250 nm.

1. filtrationAfter filtration of succinimide
2. temperaturethe filtrate was cooled in ice until crystallization
3. filtrationThe mixture is then filtered
4. customdried