反应详情

温度

50 °C

A mixture of 30.0 gm (0.118 mol) of (E)-2-[(amino)-phenylmethylene]-benzo[b]thiophen-3(2H)-one, 200 ml of glacial acetic acid and 13.5 gm (0.119 mol) of an aqueous 30% hydrogen peroxide solution was heated at 50° C. for four hours while stirring, and was then allowed to stand overnight at room temperature. After the addition of 100 ml of a 10% sodium sulfite solution, the solvent was largely distilled off in vacuo, and the residue was mixed with 300 ml of water. The solid precipitated thereby was suction-filtered off and recrystallized from ethanol/ethyl acetate (1:1 v/v) using activated charcoal. 23.0 gm (72% of theory) of light yellow crystals were obtained, m.p. 246°-247° C. (decomposition).

1. distillationthe solvent was largely distilled off in vacuo
2. additionthe residue was mixed with 300 ml of water
3. customThe solid precipitated
4. filtrationthereby was suction-filtered off
5. customrecrystallized from ethanol/ethyl acetate (1:1 v/v)
6. custom23.0 gm (72% of theory) of light yellow crystals were obtained