Methanesulfonic Acid → HCID 20634986, compound
Reaction equation
[CH3:1][O:2][C:3]1[C:8]([CH3:9])=[CH:7][C:6]([C:10]2[CH:11]=[CH:12][C:13]([N:16]3[CH2:22][CH2:21][CH2:20][N:19]([C:23]4[CH:28]=[CH:27][C:26]([C:29]5[CH:34]=[C:33]([CH3:35])[C:32]([O:36][CH3:37])=[C:31]([CH3:38])[CH:30]=5)=[CH:25][N:24]=4)[CH2:18][CH2:17]3)=[N:14][CH:15]=2)=[CH:5][C:4]=1[CH3:39].[CH3:40][S:41]([OH:44])(=[O:43])=[O:42]>CO>[CH3:40][S:41]([OH:44])(=[O:43])=[O:42].[CH3:40][S:41]([OH:44])(=[O:43])=[O:42].[CH3:37][O:36][C:32]1[C:33]([CH3:35])=[CH:34][C:29]([C:26]2[CH:27]=[CH:28][C:23]([N:19]3[CH2:20][CH2:21][CH2:22][N:16]([C:13]4[CH:12]=[CH:11][C:10]([C:6]5[CH:5]=[C:4]([CH3:39])[C:3]([O:2][CH3:1])=[C:8]([CH3:9])[CH:7]=5)=[CH:15][N:14]=4)[CH2:17][CH2:18]3)=[N:24][CH:25]=2)=[CH:30][C:31]=1[CH3:38]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of 1,4-bis[5-(4-methoxy-3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (126.0 mg, 0.240 mmol) in methanol (10 mL) was added a 1.0 M aqueous methanesulfonic acid (0.50 mL, 0.50 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (10 mL) vas added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from ethanol-diethyl ether-hexane to yield the title compound as a colorless crystalline powder (melting point: 250.0–253.0° C.) (157.0 mg, yield: 91%).
Workup
- concentrationthe reaction mixture was concentrated under reduced pressure
- additionEthanol (10 mL) vas added to the residue
- concentrationthe resulting mixture was concentrated under reduced pressure
- customThe residue was recrystallized from ethanol-diethyl ether-hexane
Sources & evidence
- ORD record
- ord-042d73f0a1fc4a8893a4fdbe551a9389
- Source dataset
- uspto-grants-2007_03
- Patent number
- US07196101B2
Reaction notes
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