反应详情

(See FIG. 10.) To a solution/slurry of thionicotinamide (3.3 g, 23.9 mmol) in ethanol (100 mL) is added chloroacetone (2.28 mL, 28.7 mmol) and the resultant slurry is heated to reflux and stirred for 48 h. The solvent was removed in vacuo and the crude material was chromatographed on silica gel (EtOAc/Hex, 50/50, Rf=0.34) to afford the title compound 26 (543 mg, 13% yield) as a brown solid: mp=42-43° C.; 1H NMR (CDCl3) δ 9.09 (m, 1H), 8.57 (m, 1H), 8.15 (m, 1H), 7.31 (m, 1H), 6.89 (m, 1H), 2.47 (s, 3E1); LRMS (ESI) calcd for C9H8N2S [M+H]+ 177. found 177.

1. temperaturethe resultant slurry is heated
2. temperatureto reflux
3. customThe solvent was removed in vacuo
4. customthe crude material was chromatographed on silica gel (EtOAc/Hex, 50/50, Rf=0.34)