Water → HCID 66915771, compound
Reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([NH:8][C:9](=[O:23])[C:10]2[CH:15]=[C:14]([N+:16]([O-])=O)[CH:13]=[CH:12][C:11]=2[NH:19][CH:20]([CH3:22])[CH3:21])[CH2:4][CH2:3]1.O>C(O)(=O)C.[Zn]>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([NH:8][C:9](=[O:23])[C:10]2[CH:15]=[C:14]([NH2:16])[CH:13]=[CH:12][C:11]=2[NH:19][CH:20]([CH3:21])[CH3:22])[CH2:6][CH2:7]1Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
2.0 g (6.5 mmol) of N-(4-methylpiperazin-1-yl)-2-isopropylamino-5-nitrobenzamide were dissolved in 40 ml of glacier acetic acid and 6.8 g of zinc powder were added gradually at 45-50° C. For workup, 40 ml of water were added, the mixture was extracted once with ethyl acetate, the water phase was alkalized with NaOH, and the mixture was extracted repeatedly with methylene chloride. The residue remaining after drying and concentration (1.9 g) could be used for the next reaction without further purification.
Workup
- extractionthe mixture was extracted once with ethyl acetate
- extractionthe mixture was extracted repeatedly with methylene chloride
- customafter drying
- concentrationconcentration (1.9 g)
- customcould be used for the next reaction without further purification
Sources & evidence
- ORD record
- ord-4f19a17c221c4ab4bcd084e3e3044679
- Source dataset
- uspto-grants-2010_07
- Patent number
- US07759379B2
Reaction notes
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