Triethylamine → HCID 14280741, Verbindung

HRID 1649777Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1649777
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH:11](O)[CH2:12][N:13]([CH2:16][CH3:17])[CH2:14][CH3:15].C(N(CC)CC)C.CS([Cl:30])(=O)=O.[F:31][C:32]1[CH:45]=[CH:44][C:35]([C:36]([CH:38]2[CH2:43][CH2:42][NH:41][CH2:40][CH2:39]2)=[O:37])=[CH:34][CH:33]=1>ClCCl.O1CCOCC1>[ClH:30].[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH:11]([N:41]1[CH2:42][CH2:43][CH:38]([C:36](=[O:37])[C:35]2[CH:34]=[CH:33][C:32]([F:31])=[CH:45][CH:44]=2)[CH2:39][CH2:40]1)[CH2:12][N:13]([CH2:16][CH3:17])[CH2:14][CH3:15]

Komponenten

7

Edukt 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 407267HCID 407267, VerbindungHCID 27244404-(4-Fluorobenzoyl)piperidine

Produkt 1

HCID 14280741HCID 14280741, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

1.4 g of 1-(2-naphthyl)-2-diethylaminoethanol was dissolved in 20 ml of dichloromethane. 2.4 ml of triethylamine and 0.9 ml of methanesulfonyl chloride were added to the solution under cooling with ice and the mixture was stirred at room temperature for 4.5 h. A solution of 1.2 g of 4-(p-fluorobenzoyl)piperidine in 25 ml of dioxane was added to the reaction mixture and the obtained mixture was refluxed for 2 h. After completion of the reaction, the product was purified according to silica gel column chromatography and then converted into its hydrochloride.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. temperaturethe obtained mixture was refluxed for 2 h
  3. customAfter completion of the reaction
  4. customthe product was purified

Quellen und Nachweise

ORD-Eintrag
ord-343a84def31d43f6be2ecd17683f8e60
Quelldatensatz
uspto-grants-1990_05
Patentnummer
US04921863

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