Methanol → HCID 13067125, compound
Reaction equation
[BH4-].[Na+].[Cl:3][C:4]1[CH:26]=[CH:25][C:7]2[C:8]3[C:9](=[C:20]([CH:23]=[O:24])[NH:21][CH:22]=3)[CH2:10][N:11]=[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:5]=1.O.[CH3:28]O>>[Cl:3][C:4]1[CH:26]=[CH:25][C:7]2[C:8]3[C:9](=[C:20]([CH2:23][OH:24])[NH:21][C:22]=3[CH3:28])[CH2:10][N:11]=[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:5]=1Participants
5
Procedure
In one portion 0.2 g (5.2 mmol) of sodium borohydride was added to 0.9 g of 8-chloro-6-(2-chlorophenyl)-2H,4H-pyrrolo[3,4-d][2]benzazepine-3-carboxaldehyde in 20 ml of methanol which was cooled to 0°. After stirring at 0° for 30 min, water was added and the resulting precipitate was collected by filtration to give a tan amorphous solid (mp 170°-180° dec.). All attempts to purify this product led to the introduction of impurities by decomposition.
Workup
- temperaturewas cooled to 0°
- filtrationthe resulting precipitate was collected by filtration
Sources & evidence
- ORD record
- ord-d6717adad52f4ab69dd6dba92874344d
- Source dataset
- uspto-grants-1984_01
- Patent number
- US04428878
Reaction notes
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