反应详情

To a solution of 1-amino-5-ethylsulfonyl-2-hydroxybenzene (20.13 g, 100.0 mmol, 1.0 equiv) in ethanol (200 mL) were added carbon disulfide (190.0 g, 150 mL, 2494 mmol, 25.0 equiv) and potassium hydroxide (6.73 g, 120 mmol, 1.2 equiv) and the reaction mixture heated to reflux over night. The solvent was evaporated, the residue treated with 1 M hydrochloric acid, extracted with ethyl acetate (3×150 mL) and the combined organic fractions dried over MgSO4. Evaporation of the organic solvent gave the crude product which was recrystallized from ethyl acetate to yield the title compound as yellowish solid. MS (ISN): 242.4 [M−H]−.

1. temperaturethe reaction mixture heated
2. temperatureto reflux over night
3. customThe solvent was evaporated
4. additionthe residue treated with 1 M hydrochloric acid
5. extractionextracted with ethyl acetate (3×150 mL)
6. dry with materialthe combined organic fractions dried over MgSO4
7. customEvaporation of the organic solvent
8. customgave the crude product which
9. customwas recrystallized from ethyl acetate