Water → HCID 86659239, compound

HRID 454658Notes

Reaction equation

HRID 454658 reaction equation
O.[CH3:2][S:3]([OH:6])(=[O:5])=[O:4].[OH:7][C:8]1[CH:31]=[CH:30][C:29]([O:32][CH2:33][CH2:34][N:35]2[CH2:40][CH2:39][N:38]([CH3:41])[CH2:37][CH2:36]2)=[CH:28][C:9]=1[C:10]([NH:12][C:13]1[CH:21]=[C:20]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:19]=[CH:18][C:14]=1[C:15]([OH:17])=[O:16])=[O:11]>O1CCCC1.C(O)C>[CH3:2][S:3]([OH:6])(=[O:5])=[O:4].[CH3:2][S:3]([OH:6])(=[O:5])=[O:4].[OH:7][C:8]1[CH:31]=[CH:30][C:29]([O:32][CH2:33][CH2:34][N:35]2[CH2:40][CH2:39][N:38]([CH3:41])[CH2:37][CH2:36]2)=[CH:28][C:9]=1[C:10]([NH:12][C:13]1[CH:21]=[C:20]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:19]=[CH:18][C:14]=1[C:15]([OH:17])=[O:16])=[O:11]

Participants

6

Reactant 3

HCID 962WaterHCID 6395Methanesulfonic AcidHCID 58508590HCID 58508590, compound

Product 1

HCID 86659239HCID 86659239, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8028TetrahydrofuranSolvent

Procedure

Water (1.0 mL), methanesulfonic acid (0.029 mL), and activated carbon (0.020 g) were added to a solution mixture of the obtained 2-(2-hydroxy-5-(2-(4-methylpiperazin-1-yl)ethoxy)benzamido)-4-phenylbenzoic acid (0.10 g) in tetrahydrofuran (2.0 mL) and ethanol (1.0 mL), followed by stirring at room temperature for 30 minutes. The insoluble substance was removed by filtration, and then the solvent was evaporated under reduced pressure. Acetone was added to the obtained residue, and the solid substance was collected by filtration to obtain 0.095 g of 2-(2-hydroxy-5-(2-(4-methylpiperazin-1-yl)ethoxy)benzamido)-4-phenylbenzoic acid dimethanesulfonate as a white solid.

Workup

  1. customThe insoluble substance was removed by filtration
  2. customthe solvent was evaporated under reduced pressure
  3. additionAcetone was added to the obtained residue
  4. filtrationthe solid substance was collected by filtration

Sources & evidence

ORD record
ord-49c23cc48b3c48f5ad114b32bd1113ba
Source dataset
uspto-grants-2013_07
Patent number
US08492582B2

Reaction notes

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