Water → HCID 86760094, compound
Reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([C:11]2[C:17]3[CH:18]=[C:19]4[O:24][CH2:23][O:22][C:20]4=[CH:21][C:16]=3[CH2:15][CH:14]([C:25]([NH2:27])=[O:26])[NH:13][N:12]=2)[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].O.[C:29](OC(=O)C)(=[O:31])[CH3:30]>>[C:29]([N:13]1[CH:14]([C:25]([NH2:27])=[O:26])[CH2:15][C:16]2[CH:21]=[C:20]3[O:22][CH2:23][O:24][C:19]3=[CH:18][C:17]=2[C:11]([C:4]2[CH:5]=[CH:6][C:7]([N+:8]([O-:10])=[O:9])=[C:2]([CH3:1])[CH:3]=2)=[N:12]1)(=[O:31])[CH3:30]Participants
4
Procedure
3.68 g (10.0 millimoles) of (±)-7,8-dihydro-5-(3-methyl-4-nitro-phenyl)-9H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-8-carboxylic acid-amide are suspended in 30 ml of acetic anhydride and stirred at room temperature for 48 hours. The reaction mixture is cooled with icecold water, the precipitated product is filtered and washed with 20 ml of diethyl ether. Thus 3.32 g of the desired compound are obtained, yield 81%, mp.: 157–161° C.
Workup
- filtrationthe precipitated product is filtered
- washwashed with 20 ml of diethyl ether
Sources & evidence
- ORD record
- ord-47a35488ca6546ca95290c52befab97d
- Source dataset
- uspto-grants-2006_05
- Patent number
- US07053082B1
Reaction notes
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