Potassium Carbonate → HCID 3082690, Verbindung

HRID 845383Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 845383
[CH3:1][C:2]1([CH3:15])[CH2:7][NH:6][C:5]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:4][CH2:3]1.F[C:17]1[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:19][C:18]=1[N+:27]([O-])=[O:28].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:1][C:2]1([CH3:15])[CH2:7][N:6]2[C:17]3[C:18]([N+:27]([O-:28])=[C:8]([C:9]4[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=4)[C:5]2=[N:4][CH2:3]1)=[CH:19][C:20]([C:23]([F:24])([F:25])[F:26])=[CH:21][CH:22]=3

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 677784-Fluoro-3-nitrobenzotrifluorideHCID 416879Pyrimidine, 1,4,5,6-tetrahydro-5,5-dimethyl-2-(phenylmethyl)-

Produkt 1

HCID 3082690HCID 3082690, VerbindungAusbeute 26,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

A mixture of 1,4,5,6-tetrahydro-5,5-dimethyl-2-phenylmethylpyrimidine (1.69, 8 mmol), 1-fluoro-2-nitro-4-trifluoromethylbenzene (1.679, 8 mmol) and potassium carbonate (550 mg, 4 mmol) in acetonitrile (25 ml) was heated overnight at 40° C. The solvent was removed in vacuo and the resulting yellow solid recrystallised from ethyl acetate to yield 2,3-dihydro-2,2-dimethyl-5-phenyl-8-trifluoromethyl-1H-pyrimido[1,2-a]quinoxaline 6-oxide (800 mg) as a yellow crystalline solid, m.p. 225°-227° C. (Found: C, 64.42, H, 4.95, N, 11.23%; C20H18F3N3O requires C, 64.34, H, 4.86, N, 11.25%) and represented by the structural formula: ##STR6##

Aufarbeitung

  1. customThe solvent was removed in vacuo
  2. customthe resulting yellow solid recrystallised from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-b9c2710a7b454dfd8efd17cf04ccf917
Quelldatensatz
uspto-grants-1988_07
Patentnummer
US04758565

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