反应详情

Combine 20 g (89.2 mmol) of the product of Example VIII with 5 g (0.16 mol) of sulfur in 250 ml of decalin and heat to 180°-190° C. under nitrogen for 7 hr. Extract the reaction with 2 liters of 2N sulfuric acid solution. Charcoal treat the extract and neutralize with potassium carbonate. Extract the aqueous portion with 800 ml of ethyl acetate, dry over magnesium sulfate, treat with charcoal, and remove the solvents under vacuum. Crystallize from ether to provide the title compound.

1. extractionExtract
2. customthe reaction with 2 liters of 2N sulfuric acid solution
3. extractionextract
4. extractionExtract the aqueous portion with 800 ml of ethyl acetate
5. dry with materialdry over magnesium sulfate
6. additiontreat with charcoal
7. customremove the solvents under vacuum
8. customCrystallize from ether