Acetonitrile → HCID 23154178, Verbindung

HRID 639443Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 639443
C(#N)C.[O:4]=[S:5]1(=[O:16])[CH2:9][CH2:8][CH2:7][N:6]1[CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.[CH3:17][O:18][C:19]1[CH:24]=[CH:23][C:22]([S:25]([N:28]2[C:32]3[CH:33]=[CH:34][C:35]([C:37]4[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=4)=[CH:36][C:31]=3[N:30]=[C:29]2Cl)(=[O:27])=[O:26])=[CH:21][CH:20]=1.C(N(C(C)C)CC)(C)C>C(OCC)(=O)C.O>[O:16]=[S:5]1(=[O:4])[CH2:9][CH2:8][CH2:7][N:6]1[CH:10]1[CH2:15][CH2:14][N:13]([C:29]2[N:28]([S:25]([C:22]3[CH:21]=[CH:20][C:19]([O:18][CH3:17])=[CH:24][CH:23]=3)(=[O:27])=[O:26])[C:32]3[CH:33]=[CH:34][C:35]([C:37]4[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=4)=[CH:36][C:31]=3[N:30]=2)[CH2:12][CH2:11]1

Komponenten

7

Edukt 4

HCID 6342AcetonitrileHCID 81531DiisopropylethylamineHCID 23154167HCID 23154167, VerbindungHCID 532560872-(piperidin-4-yl)-1lambda6,2-thiazolidine-1,1-dione

Produkt 1

HCID 23154178HCID 23154178, VerbindungAusbeute 41,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To the acetonitrile solution (3 mL) containing 4-(1,1-dioxo-1λ6-isothiazolidin-2-yl)piperidine (136 mg) were added 1-(4-methoxyphenylsulfonyl)-2-chloro-5-phenylbenzimidazole (340 mg) and diisopropylethylamine (0.41 mL), followed by stirring at room temperature for 16 hrs. The reaction mixture was diluted with ethyl acetate and water, and the organic layer was washed with an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was separated and purified on a collective thin-layer chromatograph (ethyl acetate) to give the title compound (157 mg).

Aufarbeitung

  1. washthe organic layer was washed with an aqueous saturated sodium chloride solution
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was separated
  5. custompurified on a collective thin-layer chromatograph (ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-a76bd133696a42cbab395e41794e2c15
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07691860B2

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