Sodium Bicarbonate → Suritozole
Reaktionsgleichung
[CH3:1][N:2]([C:13]([NH:15][CH3:16])=[S:14])[NH:3][C:4](=O)[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[CH:6]=1.C(=O)(O)[O-].[Na+]>>[CH3:1][N:2]1[C:13](=[S:14])[N:15]([CH3:16])[C:4]([C:5]2[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[CH:6]=2)=[N:3]1Komponenten
3
Versuchsvorschrift
2,4-Dimethyl-l-(3-fluorobenzoyl)thiosemicarbazide (11.1 g, 46.0 mmol) and 1 molar aqueous sodium bicarbonate (460 mL, 0.460 mol) were stirred and heated to reflux. After being refluxed for 5 h, the reaction was allowed to cool to room temperature. After stirring overnight, the reaction was placed in the freezer for several hours. The precipitate was then collected by filtration. Crystallization from isopropanol afforded the desired product as colorless, matted needles, mp 126°-128° C.
Aufarbeitung
- temperatureheated to reflux
- temperatureAfter being refluxed for 5 h
- waitthe reaction was placed in the freezer for several hours
- filtrationThe precipitate was then collected by filtration
- customCrystallization from isopropanol
Quellen und Nachweise
- ORD-Eintrag
- ord-4a08847f177243c6a5dbe6d3e43abe7d
- Quelldatensatz
- uspto-grants-1999_01
- Patentnummer
- US05856350
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