Methanesulfonic Acid → HCID 20634976, compound
Reaction equation
[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([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]([O:35][CH3:36])[C:32]([Cl:37])=[C:31]([O:38][CH3:39])[CH:30]=5)=[CH:25][N:24]=4)[CH2:18][CH2:17]3)=[N:14][CH:15]=2)=[CH:4][C:3]=1[O:40][CH3:41].[CH3:42][S:43]([OH:46])(=[O:45])=[O:44]>CO>[CH3:42][S:43]([OH:46])(=[O:45])=[O:44].[CH3:42][S:43]([OH:46])(=[O:45])=[O:44].[Cl:37][C:32]1[C:31]([O:38][CH3:39])=[CH:30][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:5]5[CH:6]=[C:7]([O:8][CH3:9])[C:2]([Cl:1])=[C:3]([O:40][CH3:41])[CH:4]=5)=[CH:15][N:14]=4)[CH2:17][CH2:18]3)=[N:24][CH:25]=2)=[CH:34][C:33]=1[O:35][CH3:36]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of 1,4-bis[5-(4-chloro-3,5-dimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine (130.0 mg, 0.210 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.45 mL, 0.45 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue seas recrystallized from methanol-chloroform-diethyl ether to yield the title compound as a colorless crystalline powder (melting point: 279.0–282.0° C.)(138.0 mg, yield: 83%).
Workup
- concentrationthe reaction mixture was concentrated under reduced pressure
- additionEthanol (5.0 mL) was added to the residue
- concentrationthe resulting mixture was concentrated under reduced pressure
- customThe residue seas recrystallized from methanol-chloroform-diethyl ether
Sources & evidence
- ORD record
- ord-1405845d468f437aa0879ef7c8ac9834
- Source dataset
- uspto-grants-2007_03
- Patent number
- US07196101B2
Reaction notes
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