反应详情

To 0.230 g of 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine in 3 ml of acetic acid was added 0.2 ml of concentrated sulfuric acid and, under ice-cooling, 0.3 ml of a 30% aqueous solution of hydrogen peroxide was added dropwise. The mixture was allowed to stand at 3°-5° C. for 7 hours, at the end of which time an aqueous solution of sodium sulfite was added to the mixture to decompose the excess hydrogen peroxide. The solvent was evaporated off and the residue was diluted with water. The crystals were collected by filtration. By the above procedure was obtained 3-methylsulfinyl-11H-s-triazolo[3,4-b][3]benzazepine as crystals. Recrystallization from methanol yielded colorless needles, m.p. 176°-177° C. Based on infrared absorption spectrum and other data, this compound was identified with the compound obtained in Example 17.

1. temperatureunder ice-cooling
2. customThe solvent was evaporated off
3. additionthe residue was diluted with water
4. filtrationThe crystals were collected by filtration