Hydrogen chloride-ethyl acetate → 1-(2-(4-((2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)amino)-3-fluoropiperidin-1-yl)ethyl)-7-methoxyquinoxalin-2(1H)-one hydrochloride

HRID 40003Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 40003
[O:1]1[C:10]2[CH:9]=[C:8]([CH2:11][NH:12][CH:13]3[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][N:21]4[C:30]5[C:25](=[CH:26][CH:27]=[C:28]([O:31][CH3:32])[CH:29]=5)[N:24]=[CH:23][C:22]4=[O:33])[CH2:15][CH:14]3[F:34])[N:7]=[CH:6][C:5]=2[O:4][CH2:3][CH2:2]1.[ClH:35].C(OCC)(=O)C>C(OCC)(=O)C>[ClH:35].[O:1]1[C:10]2[CH:9]=[C:8]([CH2:11][NH:12][CH:13]3[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][N:21]4[C:30]5[C:25](=[CH:26][CH:27]=[C:28]([O:31][CH3:32])[CH:29]=5)[N:24]=[CH:23][C:22]4=[O:33])[CH2:15][CH:14]3[F:34])[N:7]=[CH:6][C:5]=2[O:4][CH2:3][CH2:2]1

Komponenten

4

Versuchsvorschrift

To 2 mL of an ethyl acetate solution containing 31 mg of 1-(2-(4-((2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)amino)-3-fluoropiperidin-1-yl)ethyl)-7-methoxyquinoxalin-2(1H)-one, 0.20 mL of 4 mol/L hydrogen chloride/ethyl acetate solution was added at room temperature, and the solvent was removed under reduced pressure, diethyl ether was added and the resulting solid was filtered to give 25 mg of 1-(2-(4-((2,3-dihydro(1,4)dioxino(2,3-c)pyridin-7-ylmethyl)amino)-3-fluoropiperidin-1-yl)ethyl)-7-methoxyquinoxalin-2(1H)-one hydrochloride as a pale brown solid.

Aufarbeitung

  1. additionwas added at room temperature
  2. customthe solvent was removed under reduced pressure, diethyl ether
  3. additionwas added
  4. filtrationthe resulting solid was filtered

Quellen und Nachweise

ORD-Eintrag
ord-8482b596b5f24ea08b99024a8f0a12e9
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524738B2

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