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 2193383Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2193383
[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-fee1d068ea3a4920b0b7fb16488ecfb4
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08329694B2

Notizen zur Reaktion

Wird geladen…