反应详情

First, 2.00 g of 2-cyano-4'-methyl-1,1'-biphenyl was dissolved in a mixture of 15 ml of methanol and 4.18 g of triethylamine, and hydrogen sulfide gas was bubbled thereinto at room temperature to the point of saturation. After keeping at room temperature for 3 days, the solution was kept at 50° C. for 6 hours. The reaction mixture was concentrated under reduced pressure, and the residue was extracted with ethyl acetate containing 1% hydrochloric acid. The organic layer was concentrated to give 2.18 g of 2-thiocarbamoyl-4'-methyl-1,1'-biphenyl. Yield, 92%; m.p., 111°-115° C.; m/z, 227

1. customwas bubbled
2. customat room temperature
3. waitthe solution was kept at 50° C. for 6 hours
4. concentrationThe reaction mixture was concentrated under reduced pressure
5. extractionthe residue was extracted with ethyl acetate containing 1% hydrochloric acid
6. concentrationThe organic layer was concentrated