Triethylamine → HCID 86681323, Verbindung

HRID 1778905

Reaktionsgleichung

Reaktionsgleichung von HRID 1778905
Cl.[NH2:2][C:3]1([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.C(N(CC)CC)C.Br[CH2:22][CH2:23][O:24][CH2:25][CH2:26]Br>CN(C)C=O.C(OCC)(=O)C>[O:24]1[CH2:25][CH2:26][N:2]([C:3]2([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]2)[CH2:22][CH2:23]1

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 21521Bis(2-bromoethyl) etherHCID 11241228Ethyl 1-aminocyclohexane-1-carboxylate hydrochloride

Produkt 1

HCID 86681323HCID 86681323, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Ethyl 1-aminocyclohexancarboxylate hydrogen chloride (5.800 g), triethylamine (13.62 mL) and 1-bromo-2-(2-bromoethoxy)ethane (4.21 mL) were stirred together in N,N-dimethylformamide (50 mL) at 95° C. overnight. The reaction mixture was diluted with ethyl acetate (150 mL), washed with water (100 mL) and brine (100 mL), dried over magnesium sulfate, filtered, and concentrated. Silica gel chromatography eluting with a gradient of 5% to 25% ethyl acetate/hexanes provided the title compound.

Aufarbeitung

  1. washwashed with water (100 mL) and brine (100 mL)
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. washSilica gel chromatography eluting with a gradient of 5% to 25% ethyl acetate/hexanes

Quellen und Nachweise

ORD-Eintrag
ord-8937afdeb1bd42099cd0d560abb315d5
Quelldatensatz
uspto-grants-2016_02
Patentnummer
US09266877B2

Verknüpfte Notizen

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