反应详情

To a solution of 2.3 g. (12 mmoles) of 4-(2-amino-4-pyridyl)imidazole-2-thiol in 60 ml. of dimethylformamide was added 8 g. of Raney nickel and the mixture heated at 115° C. for 3 hours. The mixture was filtered and the filtrate concentrated to a brown solid. After trituration with boiling chloroform, the solid was taken up in 50 ml. of absolute ethanol, treated with charcoal and the filtered solution concentrated to a small volume. The precipitate was filtered and dried, 1.12 g. (60%), m.p. 193°-196° C. The analytical sample was prepared by chromatographing on Florisil TM using chloroform-methanol (9:1, v:v) as the eluent, m.p. 196°-198° C.

1. filtrationThe mixture was filtered
2. concentrationthe filtrate concentrated to a brown solid
3. additionof absolute ethanol, treated with charcoal
4. concentrationthe filtered solution concentrated to a small volume
5. filtrationThe precipitate was filtered
6. customdried
7. customThe analytical sample was prepared by chromatographing on Florisil TM