6-(2-methylpropyl)piperidine-2,4-dione → HCID 66732004, Verbindung

HRID 1963109Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1963109
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH2:7]([CH:11]1[NH:16][C:15](=O)[CH2:14][C:13](=[O:18])[CH2:12]1)[CH:8]([CH3:10])[CH3:9]>C1COCC1>[CH2:7]([CH:11]1[CH2:12][CH:13]([OH:18])[CH2:14][CH2:15][NH:16]1)[CH:8]([CH3:10])[CH3:9]

Komponenten

4

Edukt 2

HCID 52466806-(2-methylpropyl)piperidine-2,4-dioneHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 66732004HCID 66732004, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a stirred ice cooled suspension of LAH (16.1 g, 0.414 mol) in THF (100 mL), a solution of 6-isobutyl-piperidine-2,4-dione (14.0 g, 0.083 mol) in THF (100 mL) was added dropwise under N2. The reaction mixture was warmed to room temperature and stirred under N2 for 48 h. The reaction mixture was cooled to 0° C. and quenched with water (16.1 mL), 1 N NaOH (16.1 mL) and water (16.1 mL). The reaction mixture was filtered and the solid was washed with hot THF (100 mL). The filtrate was concentrated to yield 2-isobutyl-piperidin-4-ol as a solid (9 g, crude).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. customquenched with water (16.1 mL), 1 N NaOH (16.1 mL) and water (16.1 mL)
  3. filtrationThe reaction mixture was filtered
  4. washthe solid was washed with hot THF (100 mL)
  5. concentrationThe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-8dc02dea70b647bd93facac53becd429
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08415378B2

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