Propionic anhydride → HCID 18975145, compound
Reaction equation
[Br:1][C:2]1[CH:28]=[CH:27][C:5]2[CH2:6][CH:7]([CH3:26])[N:8]([C:20](=[O:25])[C:21](F)(F)F)[N:9]=[C:10]([C:11]3[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1.[C:29](OC(=O)CC)(=O)CC>>[Br:1][C:2]1[CH:28]=[CH:27][C:5]2[CH2:6][CH:7]([CH3:26])[N:8]([C:20](=[O:25])[CH2:21][CH3:29])[N:9]=[C:10]([C:11]3[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1Participants
3
Procedure
1.33 g (3.7 mmoles) of 8-bromo-4-methyl-1-(4-nitrophenyl)-3-trifluoroacetyl-4,5-dihydro-3H-2,3-benzodiazepine (prepared in Example 22, Step D) are acylated with propionic anhydride using the method of Example 1. The crude product is purified by chromatography over a silicagel column that is eluted with a mixture of hexane and ethyl acetate in a ratio of 9:1. Thus, 1.07 g (70%) of the title compound are obtained. M.p.: 178°-180° C.
Workup
- customThe crude product is purified by chromatography over a silicagel column that
- washis eluted with a mixture of hexane and ethyl acetate in a ratio of 9:1
Sources & evidence
- ORD record
- ord-f73d203829c14984a4ca5bd2259f7bbd
- Source dataset
- uspto-grants-1998_09
- Patent number
- US05807851
Reaction notes
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