Triethylamine → HCID 19045808, Verbindung

HRID 1781518Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1781518
[NH2:1][CH2:2][C:3]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:4][CH2:5][CH2:6][N:7]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:9][CH2:8]1.C(N(CC)CC)C.[CH3:38][S:39]([Cl:42])(=[O:41])=[O:40]>C(Cl)Cl>[ClH:42].[C:25]1([C:3]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)([CH2:2][NH:1][S:39]([CH3:38])(=[O:41])=[O:40])[CH2:4][CH2:5][CH2:6][N:7]2[CH2:12][CH2:11][CH:10]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:9][CH2:8]2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 9865634HCID 9865634, Verbindung

Produkt 1

HCID 19045808HCID 19045808, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 5-amino-4,4-diphenyl-1-(4-phenylpiperidino)pentane (0.4 g) and triethylamine (0.42 ml) in methylene chloride (15 ml) was added methanesulfonyl chloride (0.1 ml) dropwise under ice-cooling and stirring. After completion of dropwise addition, the mixture was returned to room temperature and stirred for another 3 hours. This reaction mixture was washed with water, dried over anhydrous sodium sulfate, and concentrated to dryness. The group was purified by silica gel column chromatography to provide the hydrochloride of the title compound (0.25 g) as colorless powder.

Aufarbeitung

  1. temperaturecooling
  2. additionAfter completion of dropwise addition
  3. customwas returned to room temperature
  4. stirringstirred for another 3 hours
  5. washThis reaction mixture was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated to dryness
  8. customThe group was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-f481802e6a614778937029828a5a0491
Quelldatensatz
uspto-grants-1997_05
Patentnummer
US05633248

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