1-Methyl-4-(nitromethyl)piperidin-4-ol → 4-(Aminomethyl)-1-methylpiperidin-4-ol

HRID 1469330

Reaktionsgleichung

Reaktionsgleichung von HRID 1469330
[CH3:1][N:2]1[CH2:7][CH2:6][C:5]([CH2:9][N+:10]([O-])=O)([OH:8])[CH2:4][CH2:3]1>C(O)C.[OH-].[Pd+2].[OH-]>[NH2:10][CH2:9][C:5]1([OH:8])[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1

Komponenten

4

Edukt 1

HCID 2733771-Methyl-4-(nitromethyl)piperidin-4-ol

Produkt 1

HCID 64842624-(Aminomethyl)-1-methylpiperidin-4-olAusbeute 106,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9942167Palladium hydroxideKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

Palladium hydroxide (2.3 g of 20% on carbon) was added to a solution of 1-methyl-4-nitromethylpiperidin-4-ol (11.57 g) in ethanol (120 mL). The mixture was placed under hydrogen pressure (50 psi, 3.4×105 Pa) on a Parr apparatus for 55 hours. The reaction mixture was filtered through a layer of CELITE filter aid and the filter cake was rinsed with methanol (100 mL). The filtrate was concentrated under reduced pressure to provide 10.18 g of 4-aminomethyl-1-methylpiperidin-4-ol as a thick oil.

Aufarbeitung

  1. customfor 55 hours
  2. filtrationThe reaction mixture was filtered through a layer of CELITE
  3. filtrationfilter aid
  4. washthe filter cake was rinsed with methanol (100 mL)
  5. concentrationThe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-1732c157d53842e9b4f3613995a655d2
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09006264B2

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