反应详情

A mixture of 2-biphenylylcyanamide (3.9 g), 4-piperidone oxime (4.5 g) and ethanol (50 ml) was stirred at ambient temperature for 6 hours and then at 50°-60° C. for 5 hours to give a brown solid which was purified by chromatography on an aluminia column eluted successively with hexane, 1:4, 2:3, 3:2 and 4:1 mixtures of dichloromethane and hexane and the 99:1 mixture of dichloromethane and methanol to yield a solid which was recrystallised from ethyl acetate to give N-(2-biphenylyl)-4-hydroxyiminopiperidine-1-carboxamidine (m.p. 175°-176° C.).

1. customat 50°-60° C. for 5 hours to give a brown solid which
2. customwas purified by chromatography on an aluminia column
3. washeluted successively with hexane, 1:4, 2:3, 3:2 and 4:1 mixtures of dichloromethane and hexane
4. additionthe 99:1 mixture of dichloromethane and methanol
5. customto yield a solid which
6. customwas recrystallised from ethyl acetate