反应详情

A solution of 2,3-dihydro-1-benzofuran-5-carbohydrazide (535 mg, 3.00 mmol), carbon disulfide (0.397 mL, 6.60 mmol) and triethylamine (0.460 mL, 3.30 mmol) in ethanol (5 mL) was heated under reflux for 24 hr. After cooling, the reaction mixture was diluted with ethyl acetate, washed with 0.1M hydrochloric acid and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from hexane/tetrahydrofuran to give the title compound (529 mg, yield 80%) as pale-yellow crystals.

1. temperatureunder reflux for 24 hr
2. temperatureAfter cooling
3. washwashed with 0.1M hydrochloric acid and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was recrystallized from hexane/tetrahydrofuran