تفاعل #54789

معادلة التفاعل

3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine

paraformaldehyde

trimethylbenzylammonium hydroxide

→

11-methylene-3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine

المذيبات

tetrahydrofuran

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter refluxing the mixture for 30 minutes
2. 2
   أخرىthe solvent was evaporated off
3. 3
   workup.ADDITIONThe residue was diluted with water
4. 4
   استخلاصextracted with ethyl acetate
5. 5
   غسيلThe ethyl acetate layer was washed with water
6. 6
   تجفيفdried over Na2SO4
7. 7
   أخرىThe solvent was then evaporated off
8. 8
   ترشيحthe residual crystals were collected by filtration
9. 9
   غسيلwashed with isopropyl alcohol
10. 10
    أخرىdried

الإجراء التجريبي

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.

المصدر