Formic Acid → 5'-fluoro-N-methyl-2'-methylsulphinylacetylformanilide

Beteiligte Stoffe

Reaktionsschritte

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.

Herkunft & Nachweise