反应详情

温度

60 °C

Chlorine (76.0 grams, 1.07 mol) was bubbled into a mechanically stirred solution of 221.0 grams (1.00 mol) of 2-(methylthiomethyl)-6-(trifluoromethyl) aniline in 2 liters of ethylene dichloride over 60 minutes while maintaining the reaction temperature below 20° C. The mixture was then heated to 60° C. while maintaining a steady stream of HCl bubbling through. Water (25 ml, 1.4 mol) was added and the HCl treatment was maintained at 60° C. for 15 minutes at which point a clear solution was obtained. Excess water was removed by azeotropic distillation (780 ml of solvent were removed) and the resulting solution was cooled to 0° C. with a steady stream of HCl bubbling through to precipitate the anilinium chloride salt. Filtration, washing of the solids with 150 ml. of cold ethylene dichloride and air-drying gave 228.0 grams (92.7%) of off-white 2-(chloromethyl)-6-(trifluoromethyl) anilinium chloride.

1. temperaturewhile maintaining the reaction temperature below 20° C
2. customwas obtained
3. customExcess water was removed by azeotropic distillation (780 ml of solvent were removed)
4. temperaturethe resulting solution was cooled to 0° C. with a steady stream of HCl bubbling through
5. customto precipitate the anilinium chloride salt
6. filtrationFiltration
7. washwashing of the solids with 150 ml
8. dry with materialof cold ethylene dichloride and air-drying