Triethylamine → HCID 20407006, Verbindung

HRID 615537Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 615537
[CH3:1][C:2]([C:5]1[CH:9]=[C:8]([NH2:10])[O:7][N:6]=1)([CH3:4])[CH3:3].C(N(CC)CC)C.[CH3:18][CH:19]([CH2:23][CH2:24][Cl:25])[C:20](Cl)=[O:21]>C(OCC)(=O)C>[Cl:25][CH2:24][CH2:23][CH:19]([CH3:18])[C:20]([NH:10][C:8]1[O:7][N:6]=[C:5]([C:2]([CH3:4])([CH3:3])[CH3:1])[CH:9]=1)=[O:21]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 20956943-Tert-butyl-1,2-oxazol-5-amineHCID 137705824-Chloro-2-methylbutanoyl chloride

Produkt 1

HCID 20407006HCID 20407006, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a stirred solution of 7 g of 3-(1,1-dimethylethyl)-5-aminoisoxazole dissolved in 50 ml ethyl acetate was added 5.05 g of triethylamine at room temperature. As the solution continued to stir, 8 g of 2-methyl-4-chlorobutyric acid chloride was added to the reaction mixture over a 15 minute period. The reaction was allowed to stir for about 3 days and the precipitated triethylamine hydrochloride salt was collected by filtration and washed with ethyl acetate. The solvent was evaporated from the filtrate under reduced pressure and the residue was recrystallized from diethyl ether to afford 4-chloro-N-[3-(1,1-dimethylethyl)-5-isoxazolyl]-2-methylbutanamide as a solid. mp 135°-137° C.

Aufarbeitung

  1. stirringto stir for about 3 days
  2. filtrationthe precipitated triethylamine hydrochloride salt was collected by filtration
  3. washwashed with ethyl acetate
  4. customThe solvent was evaporated from the filtrate under reduced pressure
  5. customthe residue was recrystallized from diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-148b9ed18c734c2f92180adc2ac95b53
Quelldatensatz
uspto-grants-1985_02
Patentnummer
US04500343

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