1,4-Dioxane hydrochloride → 1-{2-[(6-Aminohexanoyl)(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate dihydrochloride

HRID 446511Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 446511
[C:1]1([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8](=[O:35])[O:9][CH:10]1[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][N:18]([C:20](=[O:34])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH:26]C(OC(C)(C)C)=O)[CH3:19])[CH2:12][CH2:11]1.[ClH:42].O1CCOCC1>O1CCOCC1>[ClH:42].[ClH:42].[C:1]1([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8](=[O:35])[O:9][CH:10]1[CH2:11][CH2:12][N:13]([CH2:16][CH2:17][N:18]([C:20](=[O:34])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH2:26])[CH3:19])[CH2:14][CH2:15]1

Komponenten

4

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 666716851-{2-[{6-[(tert-Butoxycarbonyl)amino]hexanoyl}(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate

Produkt 1

HCID 666717251-{2-[(6-Aminohexanoyl)(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate dihydrochlorideAusbeute 105,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

The compound (1.59 g, 2.80 mmol) obtained in Example 11b was dissolved in 1,4-dioxane (7 mL), 4 N hydrochloric acid-dioxane (7.00 mL, 28.0 mmol) was added under ice cooling, and the mixture was stirred at room temperature for 20 minutes. Since insoluble material was precipitated, methanol (4 mL) was added, and the mixture was stirred at room temperature for 40 minutes. The solvent was evaporated under reduced pressure to give the title compound (1.60 g; yield, 100%) as a white solid.

Aufarbeitung

  1. customSince insoluble material was precipitated
  2. additionmethanol (4 mL) was added
  3. stirringthe mixture was stirred at room temperature for 40 minutes
  4. customThe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9cd9c3d50dab49938357f0c0383896cc
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08476253B2

Notizen zur Reaktion

Wird geladen…