Reaktionsgleichung
O.CS[C:4]1[NH:9][C:8]2[CH:10]=[CH:11][N:12]=[CH:13][C:7]=2[S:6](=[O:15])(=[O:14])[N:5]=1.[CH2:16]([NH2:19])[CH:17]=[CH2:18]>>[CH2:16]([NH:19][C:4]1[NH:9][C:8]2[CH:10]=[CH:11][N:12]=[CH:13][C:7]=2[S:6](=[O:15])(=[O:14])[N:5]=1)[CH:17]=[CH2:18]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
A mixture of 3-methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate (0.5 g) and allylamine (4 mL) was heated in a sealed bumb for 4-5 h at 120° C. After cooling, the amine was removed by distillation under reduced pressure. The residue was dissolved in 0.5N NaOH, treated with charcoal, filtered, and the filtrate was adjusted to pH 6 with 1N HCl. The resulting precipitate was collected by filtration, washed with water and dried to give the title compound as a dihydrate (yield: 0.44 g); m.p. 206°-208° C. (Compound 15).
Aufarbeitung
- temperatureAfter cooling
- customthe amine was removed by distillation under reduced pressure
- dissolutionThe residue was dissolved in 0.5N NaOH
- additiontreated with charcoal
- filtrationfiltered
- filtrationThe resulting precipitate was collected by filtration
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-085a166e785e4f3b85065ec9ad85c7db
- Quelldatensatz
- uspto-grants-1998_08
- Patentnummer
- US05792764
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