Methylamine → 5-methyl-6,7-difluoro-1H,4H-thiazolo[3,4-a]quinoxaline-1-thione
Reaktionsgleichung
Cl[CH2:2][C:3]1[N:4]([C:9]2[CH:14]=[CH:13][C:12]([F:15])=[C:11]([F:16])[C:10]=2F)[C:5](=[S:8])[S:6][CH:7]=1.[CH3:18][NH2:19]>C(#N)C.CO>[CH3:18][N:19]1[C:10]2[C:9](=[CH:14][CH:13]=[C:12]([F:15])[C:11]=2[F:16])[N:4]2[C:5](=[S:8])[S:6][CH:7]=[C:3]2[CH2:2]1Komponenten
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
4-Chloromethyl-3-(2,3,4-trifluorophenyl)-2(3H)-thiazolethione (2.5 g) prepared in the same manner as in Reference Example 7 was dissolved in acetonitrile (25 ml) and to the solution was added 40% solution of methylamine in methanol (3.3 g) and the mixture was stirred at 50° C. for 16 hours. The reaction mixture was evaporated to dryness under reduced pressure and to the residue was added water and the solution was extracted with chloroform. The extract was washed with a NaCl solution, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The obtained residue was recrystallized from a mixed solvent of cyclohexane - ethyl acetate to give the title compound (2.0 g) as pale yellow crystals, m.p. 165°-167° C.
Aufarbeitung
- customThe reaction mixture was evaporated to dryness under reduced pressure and to the residue
- additionwas added water
- extractionthe solution was extracted with chloroform
- washThe extract was washed with a NaCl solution
- dry with materialdried over anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe obtained residue was recrystallized from a mixed solvent of cyclohexane - ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-65b622811d284750b1b1fb92d8926031
- Quelldatensatz
- uspto-grants-1990_11
- Patentnummer
- US04971967
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