1-(2-(4-((3-fluoro-4-methylbenzyl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-one → 1-(2-(4-((3-fluoro-4-methylbenzyl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-one hydrochloride

HRID 2193372Notes

Reaction equation

HRID 2193372 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[CH3:30])[CH2:5][NH:6][CH:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][N:15]2[C:24]3[C:19](=[CH:20][CH:21]=[C:22]([F:25])[CH:23]=3)[N:18]=[CH:17][C:16]2=[O:26])[CH2:9][CH2:8]1.[ClH:31].C(OCC)(=O)C>C(Cl)(Cl)Cl>[ClH:31].[F:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[CH3:30])[CH2:5][NH:6][CH:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][N:15]2[C:24]3[C:19](=[CH:20][CH:21]=[C:22]([F:25])[CH:23]=3)[N:18]=[CH:17][C:16]2=[O:26])[CH2:9][CH2:8]1

Participants

4

Reactant 2

HCID 159856331-(2-(4-((3-fluoro-4-methylbenzyl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-oneHCID 21866389Hydrogen chloride-ethyl acetate

Product 1

HCID 675395301-(2-(4-((3-fluoro-4-methylbenzyl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-one hydrochloride

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

To 10 mL of a chloroform solution containing 375 mg of 1-(2-(4-((3-fluoro-4-methylbenzyl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-one, 1 mL of 4 mol/L hydrogen chloride/ethyl acetate was 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 373 mg of 1-(2-(4-((3-fluoro-4-methylbenzyl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-one hydrochloride as a pale brown solid.

Workup

  1. additionwas added
  2. customThe solvent was removed under reduced pressure, ethyl acetate
  3. additionwas added
  4. filtrationthe resulting solid was filtered

Sources & evidence

ORD record
ord-e9f95f80c1e14d7b932ccc42b4b10947
Source dataset
uspto-grants-2012_12
Patent number
US08329694B2

Reaction notes

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