Water → Bis{5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)pyrazol-4-yl}disulfide
Reaktionsgleichung
[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]2[N:23]=[CH:22][O:21][N:20]=2)[C:3]=1[S:24]C#N.[BH4-].[Na+].[OH2:29]>CO>[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:16])([F:17])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]2[N:23]=[CH:22][O:29][N:20]=2)[C:3]=1[S:24][S:24][C:3]1[C:4]([C:19]2[N:23]=[CH:22][O:21][N:20]=2)=[N:5][N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:16])([F:15])[F:17])=[CH:9][C:8]=2[Cl:18])[C:2]=1[NH2:1]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)-4-thiocyanatopyrazole 1.00 g (2.37 mmol) was dissolved in 20 ml of dry methanol, and then 210 mg (5.00 mmol) of 90% sodium borohydride was added at 0° C. After the mixture was was stirred at 0° C. for 3.5 hrs, the reaction mixture was poured into 80 ml iced water, and then the precipitate was collected by filtration. After drying in vacuo, the resulting yellow crystal was recrystalized from ethyl acetate-n-hexane mixed solvent to obtain 512 mg (0.65 mmol) of the title compound as a yellow crystal. Yield 55%.
Aufarbeitung
- filtrationthe precipitate was collected by filtration
- customAfter drying in vacuo
- customthe resulting yellow crystal was recrystalized from ethyl acetate-n-hexane mixed solvent
Quellen und Nachweise
- ORD-Eintrag
- ord-2d6dc178cc0749db85c97e55976d0047
- Quelldatensatz
- uspto-grants-2001_11
- Patentnummer
- US06316477B1
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