Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate hydrochloride → Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate

HRID 1052077

Reaktionsgleichung

Reaktionsgleichung von HRID 1052077
Cl.[CH2:2]([N:9]1[CH2:14][CH2:13][C:12](=[O:15])[CH:11]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(=O)(O)[O-].[Na+]>ClCCl>[CH2:2]([N:9]1[CH2:14][CH2:13][C:12](=[O:15])[CH:11]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:10]1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

Komponenten

4

Edukt 2

HCID 102623Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate hydrochlorideHCID 516892Sodium Bicarbonate

Produkt 1

HCID 102624Ethyl 1-benzyl-4-oxopiperidine-3-carboxylateAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

In a 5 L 3-necked flask equipped with a mechanical stirrer and a dropping funnel was placed ethyl 1-benzyl-4-oxo-3-piperidinecarboxylate hydrochloride, (199.3 g, 0.67 mol) in dichloromethane (1.5 L). To this suspension was added saturated sodium bicarbonate (1.5 L) over one hour. After the solid dissolved, the organic layer was separated, washed with brine (250 mL), filtered through 1PS filter paper and concentrated under reduced pressure to give 160.5 g (92%) of ethyl 1-benzyl-4-oxo-3-piperidinecarboxylate as an oil. NMR 60 MHz, (CDCl3), δ 7.3 (s, 5H), 4.2 (q, 2H), 3.6 (s, 2H), 2.3-3.6 (m, 6H), 1.3 (t, 3H).

Aufarbeitung

  1. customIn a 5 L 3-necked flask equipped with a mechanical stirrer and a dropping funnel
  2. dissolutionAfter the solid dissolved
  3. customthe organic layer was separated
  4. washwashed with brine (250 mL)
  5. filtrationfiltered through 1PS filter paper
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-8a209f89c3bf474fa73f7710dd3b741b
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09388176B2

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