反应详情

To p-methylthiobenzoic acid (1.68 g, 10 mmol) in THF (20 ml) were added triethylamine (1.39 ml, 10 mmol) and isobutylchloroformate (1.31 ml, 10 m). After 20 min at 20° C. ether (20 ml) was added, the mixture filtered, and hydrazine hydrate (0.49 ml, 10 mmol) added to the filtrate. After 1 h at 20° C. the solution was evaporated in vacuo and the residue recrystallised from water to give p-methylthiobenzohydrazide as short colourless needles (0.45 g, 25%); m.p. 140°-142° C.; δH (dmso-d6) 9.6 (1H, bs, NH), 7.2, 7.7 (4H, ABq, aryl), 3.8 (2H, bs, NH2), 2.5 (3H, s, sMe).

1. filtrationthe mixture filtered
2. customAfter 1 h at 20° C. the solution was evaporated in vacuo
3. customthe residue recrystallised from water