Triethylamine → HCID 86681323, Verbindung

HRID 1430296

Reaktionsgleichung

Reaktionsgleichung von HRID 1430296
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-fb5412b24ac84b32bf114eacb4a68bbe
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08940737B2

Verknüpfte Notizen

Wird geladen…