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Hydrochloric Acid → HCID 68196365, Verbindung

HRID 1626795
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1626795
[OH:1][C:2]1[C:3]([C:34]([NH:36][CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39])=[O:35])=[N:4][C:5]([CH2:9][CH:10]2[CH2:15][CH2:14][N:13]([C:16]3[CH:21]=[CH:20][C:19]([CH2:22][C:23]4[CH:28]=[CH:27][C:26]([CH2:29][O:30][CH2:31][O:32]C)=[CH:25][CH:24]=4)=[CH:18][CH:17]=3)[CH2:12][CH2:11]2)=[N:6][C:7]=1[CH3:8].Cl.O1CCOC[CH2:45]1.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[C:31]([O:30][CH2:29][C:26]1[CH:27]=[CH:28][C:23]([CH2:22][C:19]2[CH:20]=[CH:21][C:16]([N:13]3[CH2:12][CH2:11][CH:10]([CH2:9][C:5]4[N:4]=[C:3]([C:34]([NH:36][CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39])=[O:35])[C:2]([OH:1])=[C:7]([CH3:8])[N:6]=4)[CH2:15][CH2:14]3)=[CH:17][CH:18]=2)=[CH:24][CH:25]=1)(=[O:32])[CH3:45]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 68196367HCID 68196367, Verbindung

Produkt 1

HCID 68196365HCID 68196365, VerbindungAusbeute 69 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857
Ethyl Acetate
Lösungsmittel

Versuchsvorschrift

Ethyl {[(5-hydroxy-2-{[1-(4-{4-[(methoxymethoxy)methyl]benzyl}phenyl)piperidin-4-yl]methyl}-6-methylpyrimidin-4-yl)carbonyl]amino}acetate (1.1 g, 1.9 mmol) was dissolved in ethyl acetate (14 mL), and a solution of hydrogen chloride in dioxane (4 M, 7 mL, 28 mmol) was added at room temperature, followed by stirring at the same temperature for 12 hours. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction solution, followed by extraction with ethyl acetate, and subsequently the organic layer was dried over anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, the resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/ethyl acetate), and a fraction corresponding to the Rf value=0.60 (hexane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (0.74 g, 1.3 mmol) as a yellow oil (yield 69%).

Aufarbeitung

  1. extractionfollowed by extraction with ethyl acetate
  2. dry with materialsubsequently the organic layer was dried over anhydrous sodium sulfate
  3. distillationAfter the solvent was distilled off under reduced pressure
  4. customthe resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/ethyl acetate)
  5. concentrationa fraction corresponding to the Rf value=0.60 (hexane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2ef1e46930f14849a443631418b1ca26
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08785462B2

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