1-benzyl-N-methylpiperidin-4-amine → U 99363

HRID 361812

Reaktionsgleichung

Reaktionsgleichung von HRID 361812
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:17]1[C:22]([O:23][CH2:24][CH3:25])=[CH:21][CH:20]=[CH:19][N:18]=1>C(Cl)Cl>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH3:15])[C:17]2[C:22]([O:23][CH2:24][CH3:25])=[CH:21][CH:20]=[CH:19][N:18]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 41361281-benzyl-N-methylpiperidin-4-amineHCID 106319262-BROMO-3-ETHOXYPYRIDINE

Produkt 1

HCID 133107U 99363

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 1-benzyl-4-(methylamino)piperidine (EXAMPLE 9, 2.92 g) and 2-bromo-3-ethoxypyridine (EXAMPLE 69, 1.44 g) is stirred at 160°-165° in a sealed tube for 2 days, diluted with methylene chloride (50 ml), washed with water (10 ml) and saline (10 ml), dried over sodium sulfate, and concentrated under reduced pressure. The residue is chromatographed on silica gel (230-400 mesh, 300 g; eluting with a gradient of ethyl acetate/hexane (10/90-50/50)) to give the title compound, C,H,N: Anal. Calcd for C20H27N3O1 : C=73.81, H=8.36, N=12.91-found: C=73.59, H=8.37, N=12.83.

Aufarbeitung

  1. washwashed with water (10 ml) and saline (10 ml)
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue is chromatographed on silica gel (230-400 mesh, 300 g
  5. washeluting with a gradient of ethyl acetate/hexane (10/90-50/50))

Quellen und Nachweise

ORD-Eintrag
ord-f46c67e942b3493db6a54f5c40fb808f
Quelldatensatz
uspto-grants-1999_02
Patentnummer
US05866589

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