Reaktionsgleichung
[C:1](OC(=O)C)(=O)C.C(O)=O.[F:11][C:12]1[CH:17]=[CH:16][C:15]([C:18](=[O:23])[CH2:19][S:20]([CH3:22])=[O:21])=[C:14]([NH:24][CH3:25])[CH:13]=1.[OH2:26]>>[F:11][C:12]1[CH:17]=[CH:16][C:15]([C:18](=[O:23])[CH2:19][S:20]([CH3:22])=[O:21])=[C:14]([CH:13]=1)[N:24]([CH3:1])[CH:25]=[O:26]Komponenten
Versuchsvorschrift
A mixture of acetic anhydride (16.5 ml) and formic acid (11.2 ml) was stirred and heated at 50°-60° under nitrogen for 2 hours. The mixture was cooled to just below 0° and 1-(4-fluoro-2-methylaminophenyl)-2-methylsulphinylethanone (17.2 g), prepared in a similar manner to that described in Example 1, added over a period of 5 minutes. The mixture was stirred at just below 0° for 5 hours and then stored at 4° overnight. The mixture was cooled in an ice/salt bath to maintain the temperature below 0° whilst water (60 ml) was added. The mixture was evaporated in vacuo below 15° to give a green/brown oil. Purification of the oil by high performance liquid chromatography carried out using a Gilson system fitted with a 2" Dynamax silica column and eluting with dichloromethane/methanol (97.5:2.5) at 20 ml/min gave 5'-fluoro-N-methyl-2'-methylsulphinylacetylformanilide in the form of a colourless oil.
Aufarbeitung
- temperatureheated at 50°-60° under nitrogen for 2 hours
- temperatureThe mixture was cooled to just below 0°
- additionadded over a period of 5 minutes
- stirringThe mixture was stirred at just below 0° for 5 hours
- temperatureThe mixture was cooled in an ice/salt bath
- additionwas added
- customThe mixture was evaporated in vacuo below 15°
- customto give a green/brown oil
- customPurification of the oil by high performance liquid chromatography
- customfitted with a 2" Dynamax silica column
- washeluting with dichloromethane/methanol (97.5:2.5) at 20 ml/min
Quellen und Nachweise
- ORD-Eintrag
- ord-98b3ff8a3b674120bf649ccf1c84812c
- Quelldatensatz
- uspto-grants-1992_01
- Patentnummer
- US05079264
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