反应详情

A mixture of 1.1 g. (5 mmoles) of 4-(2-ethylamino-4-pyridyl)imidazole-2-thiol and 4.0 g. of Raney nickel in 30 ml. of dimethylformamide was heated at 120° C. for 4 hours. The catalysts was filtered through celite and the filtrate concentrated under reduced pressure to remove the solvent. The residual oil solidified on trituration with diethyl ether affording 830 mg. (88%) of the desired product. Purification by chromatographing over 35 g. of silica gel using chloroform-methanol (19:1, v:v) as the eluent gave 384 g. (41%) of pure product, m.p. 135°-137° C.

1. additionA mixture of 1.1 g
2. filtrationThe catalysts was filtered through celite
3. concentrationthe filtrate concentrated under reduced pressure
4. customto remove the solvent
5. customPurification by chromatographing over 35 g
6. customgave 384 g