Ammonia → HCID 13120747, compound
Reaction equation
C([O:3][C:4](=O)[CH2:5][N:6]1[CH:15]=[C:14]2[C:8]([CH2:9][N:10]=[C:11]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:12]3[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:13]=32)=[N:7]1)C.[NH3:28]>>[Cl:20][C:18]1[CH:17]=[CH:16][C:13]2[C:14]3[C:8](=[N:7][N:6]([CH2:5][C:4]([NH2:28])=[O:3])[CH:15]=3)[CH2:9][N:10]=[C:11]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[C:12]=2[CH:19]=1Participants
3
Procedure
Heating a mixture of 0.8 g (2.1 mmol) of 8-chloro-6-phenyl-2H,4H-pyrazolo[3,4-d][2]benzazepine-2-acetic acid ethyl ester and 20 ml of methanolic ammonia (ca. 20%, v/v) in an autoclave on the steam bath for 20 hr gave after crystallization from ethyl acetate/ether colorless crystals with mp 236°-238°. The analytical sample was recrystallized from ethyl acetate/methylene chloride/ether.
Workup
- temperatureHeating
- customgave
- customafter crystallization from ethyl acetate/ether colorless crystals with mp 236°-238°
- customThe analytical sample was recrystallized from ethyl acetate/methylene chloride/ether
Sources & evidence
- ORD record
- ord-7c96822ca18c47a3981ad458bf8a7ba0
- Source dataset
- uspto-grants-1984_07
- Patent number
- US04460781
Reaction notes
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