反应详情

To 0.3 g of the 1-(3-benzyl-5-methylthio-4H-1,2,4-triazol-4-yl)-2-propanone obtained in Reference Example 7 was added 15.0 g of polyphosphoric acid and the mixture was heated on an oil bath at 160°-170° C. for 4 hours. The reaction mixture was poured into ice-water, neutralized with concentrated aqueous ammonia and extracted with chloroform. The chloroform layer was washed with water and dried over Na2SO4. The solvent was evaporated off and the residue was treated with isopropyl ether. By the above procedure, 6-methyl-3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine was obtained as crystals. Recrystallization from ethyl acetate gave colorless platelets melting at 129°-130° C.

1. temperaturethe mixture was heated on an oil bath at 160°-170° C. for 4 hours
2. extractionextracted with chloroform
3. washThe chloroform layer was washed with water
4. dry with materialdried over Na2SO4
5. customThe solvent was evaporated off
6. additionthe residue was treated with isopropyl ether