Oxalyl chloride → 1-Methylpiperidine-4-carbonyl chloride hydrochloride

HRID 245714

Reaktionsgleichung

Reaktionsgleichung von HRID 245714
[ClH:1].[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([C:9](O)=[O:10])[CH2:5][CH2:4]1.C(Cl)(=O)C([Cl:15])=O>ClCCl.CN(C)C=O>[ClH:15].[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([C:9]([Cl:1])=[O:10])[CH2:5][CH2:4]1

Komponenten

5

Edukt 2

HCID 65578Oxalyl chlorideHCID 27600434-Piperidinecarboxylic acid, 1-methyl-, hydrochloride (1:1)

Produkt 1

HCID 219565061-Methylpiperidine-4-carbonyl chloride hydrochlorideAusbeute 111,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a suspension of 1-methyl-piperidine-4-carboxylic acid hydrochloride (11.36 mmol, 2.04 g) and N,N-dimethylformamide (0.129 mmol, 0.01 ml, 9.40 mg) in dichloromethane (10 ml) at 0° C. was added oxalyl chloride (14.76 mmol, 1.40 ml) drop wise. The cooling bath was removed and the reaction mixture stirred at room temperature for 20 hours. Then the reaction mixture was concentrated in vacuo to give 1-methylpiperidine-4-carbonyl chloride hydrochloride (2.5 g).

Aufarbeitung

  1. customThe cooling bath was removed
  2. concentrationThen the reaction mixture was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5c63cbcfa90a49bcbd1a3c66ee2477c2
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08658794B2

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