反应详情

温度

60 °C

Chlorine (7.60 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. A white suspension formed initially, became very thick halfway through the addition, and dissolved to give way to a cloudy solution at the end of the addition. 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. 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-trifluromethyl anilinium hydrochloride. This compound properties and analysis are described above.

1. temperaturewhile maintaining the reaction temperature below 20° C
2. customA white suspension formed initially
3. additionthrough the addition
4. dissolutiondissolved
5. customto give way to a cloudy solution
6. additionat the end of the addition
7. customwas obtained
8. customExcess water was removed by azeotropic distillation (780 ml of solvent were removed)
9. temperaturethe resulting solution was cooled to 0° C. with a steady stream of HCl bubbling through
10. filtrationFiltration
11. washwashing of the solids with 150 ml of cold ethylene dichloride
12. customair-drying