(1-methylpiperidin-4-yl)(pyridin-2-yl)methanone → HCID 131727019, Verbindung

HRID 404244Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 404244
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([C:10]2[N:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:9])[CH2:4][CH2:3]1.[ClH:16].C(O)C>C(O)C>[ClH:16].[ClH:16].[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([C:10]2[N:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:9])[CH2:4][CH2:3]1

Komponenten

4

Edukt 2

HCID 11321671(1-methylpiperidin-4-yl)(pyridin-2-yl)methanoneHCID 21887872Ethanol hydrochloride

Produkt 1

HCID 131727019HCID 131727019, VerbindungAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Resuspend the crude 2-amino-(6-(1-methylpiperidin-4-ylcarbonyl)-pyridine (14.5 g, 66.2 mmol) in ethanol (30 mL), add 2.5M HCl/ethanol (100 mL), stir the mixture for 30 minutes, and then remove the solvent under reduce pressure. Resuspend the resulting solid in 125 ml isopropanol and heat under reflux for 30 minutes. Cool the reaction mixture to room temperature, filtered-off the precipitate, rinse with 20 ml isopropanol, and dry under vacuum at 50° C. to obtain 2-amino-(6-(1-methylpiperidin-4-ylcarbonyl)-pyridine 2HCl (11 g, 63% yield corrected by HPLC % w/w).

Aufarbeitung

  1. customremove the solvent
  2. temperatureheat
  3. temperatureunder reflux for 30 minutes
  4. washfiltered-off the precipitate, rinse with 20 ml isopropanol
  5. customdry under vacuum at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-352b98cc756f418bb3de526a254e0c42
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08748459B2

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