반응 #94512

반응 방정식

end product

8-Chloro-5,6-dihydro-4-oxo-6-phenyl-4H-pyrazolo[1,5-a][1,4]benzodiazepine-2-methanol

THF

→

8-Chloro-5,6-dihydro-4-oxo-6-phenyl-4H-pyrazolo[1,5-a][1,4]benzodiazepine-2-carboxaldehyde

용매

THF hexane

반응 조건

후처리

1. 1
   온도to reflux for 17 hours
2. 2
   온도The mixture was cooled
3. 3
   여과filtered
4. 4
   세척the collected solids washed thoroughly with THF
5. 5
   농축The combined filtrate and washings were concentrated in vacuo
6. 6
   기타Recrystallization of this crude product from THF/hexane
7. 7
   기타yielded the desired end product
8. 8
   기타was obtained as colorless plate

실험 절차

A solution of 5.85 g. (17 mmol) of the end product of Example 14 in 600 ml. dry THF was mixed with 24 g. of activated MnO2 and heated to reflux for 17 hours. The mixture was cooled, filtered and the collected solids washed thoroughly with THF. The combined filtrate and washings were concentrated in vacuo. Recrystallization of this crude product from THF/hexane yielded the desired end product. An analytical sample was prepared by an additional recrystallization from THF/hexane and was obtained as colorless plate: mp 276°-278°.

출처