Reaktionsgleichung
C(N(CC)CC)C.[C:8]([NH2:14])(=[O:13])[CH2:9][C:10]([CH3:12])=[O:11].Cl[S:16](F)(=[O:18])=[O:17]>>[CH3:12][C:10]1[O:11][S:16](=[O:18])(=[O:17])[NH:14][C:8](=[O:13])[CH:9]=1Komponenten
4
Versuchsvorschrift
A mixture, with a total volume of 50 ml, of 40.4 g (0.4 mol) of triethylamine and liquid SO2 was added dropwise, at -10° C., to a solution of 20.2 g (0.2 mol) of acetoacetamide and 23.7 g (0.2 mol) of chlorosulfonyl fluoride in 70 ml of liquid SO2. The mixture was stirred for 2 hours and the liquid SO2 was then distilled off, a vacuum being applied at the end. The residue was added dropwise to 400 ml of aqueous NaOH, acidified with concentrated hydrochloric acid, with ice-cooling, and extracted with ethyl acetate. After treatment of the ethyl acetate phase with animal charcoal and Na2SO4, the extract was evaporated in vacuo. 15 g (approx. 20% of theory) of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide were obtained.
Aufarbeitung
- distillationthe liquid SO2 was then distilled off
- additionThe residue was added dropwise to 400 ml of aqueous NaOH
- temperaturecooling
- extractionextracted with ethyl acetate
- customAfter treatment of the ethyl acetate phase with animal charcoal and Na2SO4, the extract was evaporated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-35384e460b1e4317b7aa20fbd63a113b
- Quelldatensatz
- uspto-grants-1986_11
- Patentnummer
- US04625024
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