4-(Trifluoromethyl)phenyl isothiocyanate → Raf265

HRID 15092

Reaktionsgleichung

Reaktionsgleichung von HRID 15092
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:8]=[CH:7][C:6]([N:9]=[C:10]=S)=[CH:5][CH:4]=1.[F:14][C:15]([F:38])([F:37])[C:16]1[NH:20][C:19]([C:21]2[CH:26]=[C:25]([O:27][C:28]3[CH:29]=[C:30]([NH2:36])[C:31]([NH:34][CH3:35])=[CH:32][CH:33]=3)[CH:24]=[CH:23][N:22]=2)=[N:18][CH:17]=1.NC(N)=S>C(#N)C.O=P(Cl)(Cl)Cl>[CH3:35][N:34]1[C:31]2[CH:32]=[CH:33][C:28]([O:27][C:25]3[CH:24]=[CH:23][N:22]=[C:21]([C:19]4[NH:20][C:16]([C:15]([F:37])([F:14])[F:38])=[CH:17][N:18]=4)[CH:26]=3)=[CH:29][C:30]=2[N:36]=[C:10]1[NH:9][C:6]1[CH:7]=[CH:8][C:3]([C:2]([F:13])([F:12])[F:1])=[CH:4][CH:5]=1

Komponenten

6

Edukt 3

HCID 1371344-(Trifluoromethyl)phenyl isothiocyanateHCID 2723790ThioureaHCID 575318901,2-Benzenediamine,n1-methyl-4-[[2-[5-(trifluoromethyl)-1h-imidazol-2-yl]-4-pyridinyl]oxy]-

Produkt 1

HCID 11656518Raf265

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 24813Phosphorus oxychlorideLösungsmittel

Versuchsvorschrift

4-Trifluoromethylphenyl isothiocyanate (200 mg, 1 mmol) was added to a mixture of 4-(2-(5-(trifluoromethyl)-1H-imidazol-2-yl)pyridin-4-yloxy)-N1-methylbenzene-1,2-diamine (350 mg, 1 mmol) in 3 mL of acetonitrile. After stirring for 20 min at ambient temperature, HPLC analysis showed complete conversion. A mixture of thiourea (553 mg, 1 mmol) in POCl3 (3 mL) was stirred at ambient temperature. After 4 h, the mixture was heated to approximately 50° C. After heating for 2 h, HPLC analysis indicated completion of reaction:

Aufarbeitung

  1. stirringwas stirred at ambient temperature
  2. waitAfter 4 h
  3. temperaturethe mixture was heated to approximately 50° C
  4. temperatureAfter heating for 2 h
  5. customcompletion of reaction

Quellen und Nachweise

ORD-Eintrag
ord-d874d789a81547719f2e9f1c4c305bff
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07732465B2

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