HCID 57633726, Verbindung → HCID 57633720, Verbindung

HRID 2240884Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2240884
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]([CH2:15][C:16](=[CH2:21])[C:17]([O:19][CH3:20])=[O:18])[CH2:10][C:11]([F:14])([F:13])[F:12])=[CH:5][C:4]=1[C:22]([F:25])([F:24])[F:23])#[N:2]>CCOC(C)=O.[Pd]>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]([CH2:10][C:11]([F:14])([F:13])[F:12])[CH2:15][CH:16]([CH3:21])[C:17]([O:19][CH3:20])=[O:18])=[CH:5][C:4]=1[C:22]([F:23])([F:25])[F:24])#[N:2]

Komponenten

4

Edukt 1

HCID 57633726HCID 57633726, Verbindung

Produkt 1

HCID 57633720HCID 57633720, VerbindungAusbeute 62,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

A suspension of 5% Pd/C (0.060 g) in EtOAc (3 mL) was stirred under an H2 atmosphere (balloon pressure) for 15 min. A solution of methyl 2-{[[4-cyano-3-(trifluoromethyl)phenyl](2,2,2-trifluoroethyl)amino]methyl}acrylate (0.090 g, 0.245 mmol) in EtOAc (3 mL) was added and the mixture stirred for 1 hr. The catalyst was filtered off and washed with EtOAc. The filtrate was concentrated and purified by silica gel chromatography to afford 0.056 g (62% yield) of the title compound: MS (ES) m/z 369 (M+1).

Aufarbeitung

  1. stirringthe mixture stirred for 1 hr
  2. filtrationThe catalyst was filtered off
  3. washwashed with EtOAc
  4. concentrationThe filtrate was concentrated
  5. custompurified by silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-8533fa2d3fca43ac8a3913f752502895
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07723385B2

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