反应详情

A suspension of benzothiazole-6-carbohydrazide trifluoroacetate (4.92 g, 16.0 mmol), carbon disulfide (2.41 mL, 40.0 mmol) and triethylamine (5.58 mL, 40.0 mmol) in ethanol (60 mL) was heated under reflux for 1.5 hr. After cooling, the reaction mixture was diluted with ethyl acetate/tetrahydrofuran, washed with 1M hydrochloric acid and water, and concentrated under reduced pressure. The residue was recrystallized from tetrahydrofuran to give the title compound (3.11 g, yield 83%) as pale-yellow crystals.

1. temperaturewas heated
2. temperatureunder reflux for 1.5 hr
3. temperatureAfter cooling
4. washwashed with 1M hydrochloric acid and water
5. concentrationconcentrated under reduced pressure
6. customThe residue was recrystallized from tetrahydrofuran