تفاعل #94509

معادلة التفاعل

end product

8-Chloro-6-phenyl-4H-pyrazolo[1,5-a][1,4]benzodiazepine-2-carboxylic acid, methyl ester

ammonia

→

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

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe glass bomb was then sealed
2. 2
   درجة الحرارةthe reaction heated to 70°
3. 3
   درجة الحرارةAfter cooling to 5°
4. 4
   تركيزflask and concentrated in vacuo
5. 5
   أخرىRecrystallization
6. 6
   أخرىAn analytical sample was prepared by an additional recrystallization from acetone/hexane
7. 7
   أخرىobtained as pale yellow needles

الإجراء التجريبي

A solution of 750 mg. (2.13 mmol) of the end product of Example 9 in 50 ml. methanol in a glass bomb was cooled to 3° and saturated with ammonia. The glass bomb was then sealed and the reaction heated to 70° with stirring, for 16 hours. After cooling to 5°, the bomb was opened, the contents transferred to a r.b. flask and concentrated in vacuo. Recrystallization was acetone/hexane yielded end product, mp 216°-218°. An analytical sample was prepared by an additional recrystallization from acetone/hexane and obtained as pale yellow needles: mp 217°-219°.

المصدر