反应详情

To the solution of product from step A is added 2 g. of dinitrogen tetraoxide dissolved in dichloromethane, and the mixture is stirred for about 16 hours. Evaporation provides a residue which is mixed with ice and 10 percent sodium hydroxide solution. The mixture is stirred for 15 minutes, then cold 6N hydrochloric acid and diethyl ether are added. The ether layer is separated, then washed with saturated sodium chloride solution and dried. The solution is chromatographed on silica gel, eluting first with carbon tetrachloride, then dichloromethane. The later fractions are evaporated to provide 1-(2-nitro-3-phenyl-5-benzofuranyl)undecan-1-ol as a yellow solid, m.p. 84°-85° C. after recrystallization from hexane.

1. customEvaporation
2. customprovides a residue which
3. stirringThe mixture is stirred for 15 minutes
4. customThe ether layer is separated
5. washwashed with saturated sodium chloride solution
6. customdried
7. customThe solution is chromatographed on silica gel
8. washeluting first with carbon tetrachloride
9. customThe later fractions are evaporated