反应详情

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.

1. temperatureheated at 50°-60° under nitrogen for 2 hours
2. temperatureThe mixture was cooled to just below 0°
3. additionadded over a period of 5 minutes
4. stirringThe mixture was stirred at just below 0° for 5 hours
5. temperatureThe mixture was cooled in an ice/salt bath
6. additionwas added
7. customThe mixture was evaporated in vacuo below 15°
8. customto give a green/brown oil
9. customPurification of the oil by high performance liquid chromatography
10. customfitted with a 2" Dynamax silica column
11. washeluting with dichloromethane/methanol (97.5:2.5) at 20 ml/min