Ethyl Acetoacetate → HCID 178471725, Verbindung

HRID 255398

Reaktionsgleichung

Reaktionsgleichung von HRID 255398
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].[F:10][C:11]([F:15])([F:14])[C:12]#[N:13]>CC(C)([O-])C.[K+]>[C:3]([C:2](=[C:12]([NH2:13])[C:11]([F:15])([F:14])[F:10])[C:1]([O:7][CH2:8][CH3:9])=[O:6])(=[O:4])[CH3:5]

Komponenten

4

Edukt 2

HCID 8868Ethyl AcetoacetateHCID 67710Trifluoroacetonitrile

Produkt 1

HCID 178471725HCID 178471725, VerbindungAusbeute 62 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23665647Potassium tert-butoxideKatalysator

Versuchsvorschrift

To a 1 liter, four-necked flask equipped with nitrogen inlet, thermometer, and mechanical stirrer was charged 499.74 g (490 ml, 3.84 mol) of ethyl acetoacetate and 12.9 g (0.115 mol) of potassium-t-butoxide. The resulting mixture was stirred while 391 g (4.04 mol) of trifluoroaceto-nitrile was added. The reaction mixture was washed with hexane and the resulting solid was dried in vacuo affording 535 g (62%) of the enamine as a yellow solid; mp 63°-65° C.

Aufarbeitung

  1. customTo a 1 liter, four-necked flask equipped with nitrogen inlet
  2. additionwas added
  3. washThe reaction mixture was washed with hexane
  4. customthe resulting solid was dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-60f8f45313854275aba8a55ac21693a9
Quelldatensatz
uspto-grants-1987_10
Patentnummer
US04698093

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