Methanesulfonic Acid → HCID 22485476, compound
Reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13]2[CH:18]=[CH:17][C:16]([NH:19][CH2:20][CH2:21][O:22][CH2:23][CH2:24][NH:25][C:26]3[CH:27]=[CH:28][C:29]([C:32]4[CH:37]=[C:36]([O:38][CH3:39])[C:35]([O:40][CH3:41])=[C:34]([O:42][CH3:43])[CH:33]=4)=[N:30][CH:31]=3)=[CH:15][N:14]=2)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[CH3:44][S:45]([OH:48])(=[O:47])=[O:46]>C(O)C>[CH3:44][S:45]([OH:48])(=[O:47])=[O:46].[CH3:44][S:45]([OH:48])(=[O:47])=[O:46].[CH3:39][O:38][C:36]1[CH:37]=[C:32]([C:29]2[CH:28]=[CH:27][C:26]([NH:25][CH2:24][CH2:23][O:22][CH2:21][CH2:20][NH:19][C:16]3[CH:17]=[CH:18][C:13]([C:5]4[CH:6]=[C:7]([O:11][CH3:12])[C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=4)=[N:14][CH:15]=3)=[CH:31][N:30]=2)[CH:33]=[C:34]([O:42][CH3:43])[C:35]=1[O:40][CH3:41]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of bis[N-[2-(3,4,5-trimethoxyphenyl)-5-pyridyl]-2-aminoethyl]ether (53.1 mg, 0.0900 mmol) in ethanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid solution (0.20 mL, 0.20 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (10 mL) was added to the residue, and the mixture was concentrated under reduced pressure. The residue was suspended in ethanol-diethyl ether and the resulting precipitate was collected by filtration to provide the title compound as a pale brown amorphous powder (49.9 mg, yield: 71%).
Workup
- concentrationthe reaction mixture was concentrated under reduced pressure
- additionEthanol (10 mL) was added to the residue
- concentrationthe mixture was concentrated under reduced pressure
- filtrationthe resulting precipitate was collected by filtration
Sources & evidence
- ORD record
- ord-5253ddeb7ecc4936b2822ab0307cd2ad
- Source dataset
- uspto-grants-2005_05
- Patent number
- US06890940B2
Reaction notes
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