反应详情

A mixture of 1-(4-fluoro-2-methylaminophenyl)-2-methylsulphinylethanone (100 g), prepared in a similar manner to that described in Example 1, sodium hydrogen sulphite (1 kg) and water (2.5 1) was stirred under nitrogen and heated at 90°-105° for 3 hours. The mixture was allowed to cool and then stood at ambient temperature for 72 hours. The mixture was extracted with dichloromethane (3×250 ml) and the combined extracts evaporated to give a solid product. Crystallisation from hexane gave 1-(4-fluoro-2-methylaminophenyl)-2-(methylthio)ethanone, m.p. 61.5°-63°.

1. customprepared in a similar manner to that
2. temperatureheated at 90°-105° for 3 hours
3. temperatureto cool
4. extractionThe mixture was extracted with dichloromethane (3×250 ml)
5. customthe combined extracts evaporated
6. customto give a solid product
7. customCrystallisation from hexane