Diisopropylethylamine → HCID 68289892, Verbindung

HRID 68765

Reaktionsgleichung

Reaktionsgleichung von HRID 68765
[CH3:1][C:2]1[N:3]=[CH:4][O:5][C:6]=1[C:7]1[CH:15]=[CH:14][C:10]([C:11](Cl)=[O:12])=[CH:9][CH:8]=1.[C:16]([O:20][C:21]([N:23]1[CH2:28][CH2:27][CH:26]([NH:29][CH:30]2[CH2:32][CH2:31]2)[CH2:25][CH2:24]1)=[O:22])([CH3:19])([CH3:18])[CH3:17].C(N(C(C)C)C(C)C)C>ClCCl>[C:16]([O:20][C:21]([N:23]1[CH2:28][CH2:27][CH:26]([N:29]([CH:30]2[CH2:31][CH2:32]2)[C:11](=[O:12])[C:10]2[CH:14]=[CH:15][C:7]([C:6]3[O:5][CH:4]=[N:3][C:2]=3[CH3:1])=[CH:8][CH:9]=2)[CH2:25][CH2:24]1)=[O:22])([CH3:19])([CH3:17])[CH3:18]

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 2769591tert-Butyl 4-(cyclopropylamino)piperidine-1-carboxylateHCID 86678211HCID 86678211, Verbindung

Produkt 1

HCID 68289892HCID 68289892, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

4-(4-Methyl-oxazol-5-yl)-benzoyl chloride (340 mg) is added portionwise to a mixture of 4-cyclopropylamino-piperidine-1-carboxylic acid tert-butyl ester (369 mg) and ethyldiisopropylamine (274 μL) in dichloromethane (10 mL). The mixture is stirred for 1 h at room temperature, washed with water, aqueous citric acid solution and 0.5 M NaOH, dried over Na2SO4 and concentrated in vacuo. The residue is chromatographed on silica gel (dichloromethane/methanol 50:1) to afford the title compound. Mass spectrum (ESI+): m/z=426 [M+H]+.

Aufarbeitung

  1. washwashed with water, aqueous citric acid solution and 0.5 M NaOH
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe residue is chromatographed on silica gel (dichloromethane/methanol 50:1)

Quellen und Nachweise

ORD-Eintrag
ord-c5f1f69d065c44b5a1fb053cecec2fd0
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822471B2

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