反应详情

A mixture of 2-biphenylylcyanamide (4 g), 3-hydroxypiperidine (2.5 g) and ethanol (30 ml) was heated at 90°-95° C. for 8 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 then a 99:1 mixture of dichloromethane and methanol to yield a solid which was recrystallised from ethyl acetate to give N-(2-biphenylyl)-3-hydroxypiperidine-1-carboxamidine (m.p. 144°-145° C.).

1. temperaturewas heated at 90°-95° C. for 8 hours
2. customto give a brown solid which
3. customwas purified by chromatography on an aluminia column
4. washeluted successively with hexane, 1:4, 2:3, 3:2 and 4:1 mixtures of dichloromethane and hexane
5. additiona 99:1 mixture of dichloromethane and methanol
6. customto yield a solid which
7. customwas recrystallised from ethyl acetate