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4-(2-Methylphenyl)piperidine hydrochloride → HCID 23157114, Verbindung

HRID 2265161
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2265161
[CH2:1]=[C:2]1[C:8](=[O:9])[NH:7][C:6]2[N:10]=[CH:11][CH:12]=[CH:13][C:5]=2[CH2:4][CH2:3]1.Cl.[C:15]1([CH3:27])[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>CN(C)C=O>[C:15]1([CH3:27])[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH:21]1[CH2:26][CH2:25][N:24]([CH2:1][CH:2]2[C:8](=[O:9])[NH:7][C:6]3[N:10]=[CH:11][CH:12]=[CH:13][C:5]=3[CH2:4][CH2:3]2)[CH2:23][CH2:22]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 219369564-(2-Methylphenyl)piperidine hydrochlorideHCID 231570067-methylene-5,6,7,9-tetrahydro-8H-pyrido[2,3-b]azepin-8-one

Produkt 1

HCID 23157114HCID 23157114, VerbindungAusbeute 36,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

15 mg of the compound obtained in Production Example 5 was added to N,N-dimethylformamide (2 mL) solution of 19.7 mg of the compound obtained in Production Example 48, and stirred overnight at 90° C. Water was added to the reaction liquid, and extracted with ethyl acetate. The ethyl acetate layer was dried with anhydrous sodium sulfate, the solvent was evaporated off under reduced pressure, and the residue was separated and purified through preparative thin-layer chromatography (chloroform/methanol 4/1) to obtain 1.2 mg of the entitled compound and 16.6 mg of 7-methylene-5,6,7,9-tetrahydro-8H-pyrido[2,3-b]azepin-8-one. 16.6 mg of the obtained 7-methylene-5,6,7,9-tetrahydro-8H-pyrido[2,3-b]azepin-8-one was dissolved in 2 mL of N,N-dimethylformamide, and 20 mg of 4-o-tolylpiperidine monohydrochloride was added thereto and stirred at 90° C. for 0.5 hours. The reaction solution was concentrated under reduced pressure, and the residue was separated and purified through preparative thin-layer chromatography (chloroform/methanol=4/1) to obtain 12.1 mg of the entitled compound.

Aufarbeitung

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. customthe residue was separated
  3. custompurified through preparative thin-layer chromatography (chloroform/methanol=4/1)

Quellen und Nachweise

ORD-Eintrag
ord-2f9665547ccf4c81a97d40919f34b133
Quelldatensatz
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07855294B2

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