تفاعل #323906

معادلة التفاعل

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

المذيبات

THF hexane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto reflux for 17 hours
2. 2
   درجة الحرارةThe mixture was cooled
3. 3
   ترشيحfiltered
4. 4
   غسيلthe collected solids washed thoroughly with THF
5. 5
   تركيزThe combined filtrate and washings were concentrated in vacuo
6. 6
   أخرىRecrystallization of this crude product from THF/hexane
7. 7
   أخرىyielded the desired end product
8. 8
   أخرىwas obtained as colorless plates

الإجراء التجريبي

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 plates: mp 276°-278°.

المصدر