反应详情

To 4.6 g of 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine in 60 ml of tetrahydrofuran was added 2.4 g of paraformaldehyde together with 4.0 ml of a 40% solution of trimethylbenzylammonium hydroxide in methanol. After refluxing the mixture for 30 minutes, the solvent was evaporated off. The residue was diluted with water and extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over Na2SO4. The solvent was then evaporated off and the residual crystals were collected by filtration, washed with isopropyl alcohol and dried. The above procedure provided 11-methylene-3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine as crystals. Recrystallization from ethyl acetate yielded colorless needles melting at 121°-122° C.

1. temperatureAfter refluxing the mixture for 30 minutes
2. customthe solvent was evaporated off
3. additionThe residue was diluted with water
4. extractionextracted with ethyl acetate
5. washThe ethyl acetate layer was washed with water
6. dry with materialdried over Na2SO4
7. customThe solvent was then evaporated off
8. filtrationthe residual crystals were collected by filtration
9. washwashed with isopropyl alcohol
10. customdried