Methanesulfonic Acid → HCID 86659240, compound
Reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].O1CCCC1.[CH2:11]([N:13]1[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][O:21][C:22]2[CH:23]=[CH:24][C:25]([OH:46])=[C:26]([CH:45]=2)[C:27]([NH:29][C:30]2[CH:38]=[C:37]([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)[CH:36]=[CH:35][C:31]=2[C:32]([OH:34])=[O:33])=[O:28])[CH2:15][CH2:14]1)[CH3:12]>C(O)C>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH2:11]([N:13]1[CH2:14][CH2:15][N:16]([CH2:19][CH2:20][O:21][C:22]2[CH:23]=[CH:24][C:25]([OH:46])=[C:26]([CH:45]=2)[C:27]([NH:29][C:30]2[CH:38]=[C:37]([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)[CH:36]=[CH:35][C:31]=2[C:32]([OH:34])=[O:33])=[O:28])[CH2:17][CH2:18]1)[CH3:12]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
Methanesulfonic acid (0.027 mL), tetrahydrofuran (3.0 mL), and activated carbon (0.020 g) were added to an ethanol (2.0 mL) suspension of the obtained 2-(5-(2-(4-ethylpiperazin-1-yl)ethoxy)-2-hydroxybenzamido)-4-phenylbenzoic acid (0.10 g), followed by stirring at room temperature for 30 minutes. The insoluble substance was removed by filtration, and the solvent was evaporated under reduced pressure. Acetone was added to the obtained residue, and the solid substance was collected by filtration to obtain 0.090 g of 2-(5-(2-(4-ethylpiperazin-1-yl)ethoxy)-2-hydroxybenzamido)-4-phenylbenzoic acid dimethanesulfonate as a white solid.
Workup
- customThe insoluble substance was removed by filtration
- customthe solvent was evaporated under reduced pressure
- additionAcetone was added to the obtained residue
- filtrationthe solid substance was collected by filtration
Sources & evidence
- ORD record
- ord-74951d028ac145a49eaec39178c302af
- Source dataset
- uspto-grants-2013_07
- Patent number
- US08492582B2
Reaction notes
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