反应详情

An ethyl 4-methylbenzoate (EMB) solution (1134 g in chlorobenzene (CB), ~43 wt. %, 2.93 mol) was charged into a 2-Liter round bottomed flask equipped with mechanical stirrer (300 RPM stirring rate) and a cooling condenser, and heated. The temperature controller was set at 140° C., and a scrubber was connected to the condenser. Liquid bromine (275 g, 1.72 mol or ~59 mol %, Aldrich, 99.5+%, A.C.S. reagent) was fed via Viton tubings, and the bromine feed rate was adjusted to 1.00 mL/minute for the first 30 mol % of bromine and then to 0.50 mL/minute for the rest of the addition at 140° C. Heating and stirring was continued for a few minutes after all bromine was added and the hot mixture was purged with nitrogen for 20 minutes, then allowed to cool to obtain 1183 g crude reaction mixture (some materials were used for routine analysis). The GC wt. % analysis of the crude reaction mixture indicated the following:

1. customequipped with mechanical stirrer
2. temperatureheated
3. customwas set at 140° C.
4. additionto 0.50 mL/minute for the rest of the addition at 140° C
5. temperatureHeating
6. stirringstirring
7. waitwas continued for a few minutes
8. customthe hot mixture was purged with nitrogen for 20 minutes
9. temperatureto cool
10. customto obtain 1183 g crude
11. customreaction mixture (some materials
12. customThe GC wt. % analysis of the crude reaction mixture