Hydrogen chloride-ethyl acetate → 1-(2-(4-((7-bromo-2,3-dihydro-1,4-benzodioxin-6-yl)methylamino)piperidin-1-yl)ethyl)-7-methoxyquinoxalin-2(1H)-one hydrochloride
Reaction equation
[Br:1][C:2]1[C:3]([CH2:12][NH:13][CH:14]2[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][N:22]3[C:31]4[C:26](=[CH:27][CH:28]=[C:29]([O:32][CH3:33])[CH:30]=4)[N:25]=[CH:24][C:23]3=[O:34])[CH2:16][CH2:15]2)=[CH:4][C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1.[ClH:35].C(OCC)(=O)C>C(Cl)(Cl)Cl>[ClH:35].[Br:1][C:2]1[C:3]([CH2:12][NH:13][CH:14]2[CH2:15][CH2:16][N:17]([CH2:20][CH2:21][N:22]3[C:31]4[C:26](=[CH:27][CH:28]=[C:29]([O:32][CH3:33])[CH:30]=4)[N:25]=[CH:24][C:23]3=[O:34])[CH2:18][CH2:19]2)=[CH:4][C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
101 mg of 1-(2-(4-((7-bromo-2,3-dihydro-1,4-benzodioxin-6-yl)methylamino)piperidin-1-yl)ethyl)-7-methoxyquinoxalin-2(1H)-one was dissolved in 3 mL of chloroform, 0.5 mL of 4 mol/L hydrogen chloride/ethyl acetate and 3 mL of chloroform were added, and stirred at room temperature for 10 min. The solvent was removed under reduced pressure, ethyl acetate was added and the resulting solid was filtered to give 92 mg of 1-(2-(4-((7-bromo-2,3-dihydro-1,4-benzodioxin-6-yl)methylamino)piperidin-1-yl)ethyl)-7-methoxyquinoxalin-2(1H)-one hydrochloride as a dark brown powder.
Workup
- customThe solvent was removed under reduced pressure, ethyl acetate
- additionwas added
- filtrationthe resulting solid was filtered
Sources & evidence
- ORD record
- ord-5605afb9608a47eb84313167be8fc154
- Source dataset
- uspto-grants-2013_09
- Patent number
- US08524738B2
Reaction notes
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