Methyl iodide → HCID 9938497, Verbindung

HRID 565928Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 565928
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([NH:20][C:21]4[CH:26]=[CH:25][C:24]([CH2:27][N:28]5[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]5)=[CH:23][CH:22]=4)=[O:19])=[CH:13][C:12]=3[CH:34]=2)=[CH:4][CH:3]=1.[CH3:35][I:36]>CN(C)C=O>[I-:36].[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([NH:20][C:21]4[CH:22]=[CH:23][C:24]([CH2:27][N+:28]5([CH3:35])[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]5)=[CH:25][CH:26]=4)=[O:19])=[CH:13][C:12]=3[CH:34]=2)=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 6328Methyl iodideHCID 3013432HCID 3013432, Verbindung

Produkt 1

HCID 9938497HCID 9938497, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 7-(4-methylphenyl)-N-(4-(piperidinomethyl)-phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (1.4g) and methyl iodide (0.58ml) in dimethylformamide (50ml) was stirred at room temperature over night. The solvent was evaporated, and to the residue was added ethyl acetate. Precipitated crude crystal was filtered, which were recrystallized from ethanol-ethyl acetate to give 1-(N-(7-(4-methylphenyl)-2,3-dihydro-1-benzoxepin-4carbonyl)-4-aminobenzyl)-1-methylpiperidinium iodide (Compound 96) (1.6g) as colorless crystals.

Aufarbeitung

  1. customThe solvent was evaporated
  2. additionto the residue was added ethyl acetate
  3. customPrecipitated crude crystal
  4. filtrationwas filtered
  5. customwhich were recrystallized from ethanol-ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-4c284e7846354535a77d97f2b283e977
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06172061B2

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