反应详情

温度

0 °C

5 g (27.64 mmol) of 4-fluoro-2-(trifluoromethyl)-aniline is dissolved in 25 ml of dry pyridine and the solution is cooled to 0° C. A solution of 4.82 g (27.4 mmol) of chlorosulfonyl acetic acid methyl ester in 20 ml of dichloromethane is instilled in the cooled solution in the course of about 10 minutes with the temperature being maintained. Then it is stirred for 6 hours at room temperature. The reaction solution is then diluted with 100 ml of dichloromethane, the pyridine is shaken out with 2N hydrochloric acid, the organic phase is dried on magnesium sulfate, filtered and evaporated to dryness. The residue is crystallized from diethyl ether/hexane yield is obtained as a crystallizate. Melting point 84°-86° C.

1. customis instilled in the cooled solution in the course of about 10 minutes with the temperature
2. temperaturebeing maintained
3. customthe organic phase is dried on magnesium sulfate
4. filtrationfiltered
5. customevaporated to dryness
6. customThe residue is crystallized from diethyl ether/hexane
7. customyield
8. customis obtained as a crystallizate