Acetic Anhydride → HCID 178474989, Verbindung

HRID 278616

Reaktionsgleichung

Reaktionsgleichung von HRID 278616
Cl.[NH2:2][C@H:3]1[CH2:8][CH2:7][C@H:6]([C:9]([N:11]2[CH2:16][CH2:15][N:14]([S:17]([C:20]3[CH:29]=[CH:28][C:27]4[C:22](=[CH:23][CH:24]=[C:25]([Cl:30])[CH:26]=4)[CH:21]=3)(=[O:19])=[O:18])[CH2:13][CH2:12]2)=[O:10])[CH2:5][CH2:4]1.C(N(CC)CC)C.[C:38](OC(=O)C)(=[O:40])[CH3:39]>ClCCl>[C:38]([NH:2][C@H:3]1[CH2:8][CH2:7][C@H:6]([C:9]([N:11]2[CH2:12][CH2:13][N:14]([S:17]([C:20]3[CH:29]=[CH:28][C:27]4[C:22](=[CH:23][CH:24]=[C:25]([Cl:30])[CH:26]=4)[CH:21]=3)(=[O:18])=[O:19])[CH2:15][CH2:16]2)=[O:10])[CH2:5][CH2:4]1)(=[O:40])[CH3:39]

Komponenten

5

Edukt 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 178479260HCID 178479260, Verbindung

Produkt 1

HCID 178474989HCID 178474989, VerbindungAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 1-(trans-4-aminocyclohexane-1-ylcarbonyl)-4-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride (50 mg) and triethylamine (30 mg) in dichloromethane (10 ml) was added acetic anhydride (50 mg), and the mixture was stirred at room temperature for 3 hours. The reaction solution was concentrated, and the residue was purified with silica gel column chromatography (ethyl acetate) to give colorless crystals of the title compound (41 mg).

Aufarbeitung

  1. concentrationThe reaction solution was concentrated
  2. customthe residue was purified with silica gel column chromatography (ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-689c823ebf1c464eb6ae440fd04c6302
Quelldatensatz
uspto-grants-2002_03
Patentnummer
US06359134B1

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