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ChemicalBook CAS DataBase List 4-Amino-3,5-dichlorobenzotrifluoride

4-Amino-3,5-dichlorobenzotrifluoride synthesis

13synthesis methods
-

Yield:24279-39-8 98% ,39885-50-2 0.09%

Reaction Conditions:

with chlorine in chlorobenzene at 110; for 6.5 h;

Steps:

Preparation of 98% 2,6-dichloro-para-trifluoromethyIaniline

12 140 kg of pure monochlorobenzene are charged to a 20 m3 jacketed reactor rendered inert with nitrogen. The solvent heel is subsequently brought to 110C by heating the jacket. The reactor is subsequently fed with a 70% solution of para-trifluoromethylaniline in monochlorobenzene at a flow rate of 792 kg/h for 6 h 30 and with Cl at a flow rate of 488 kg/h. The temperature is maintained at 110C by cooling the jacket. Once feeding is complete, the residual content of para-trifluoromethylaniline or of monochloro derivative is monitored. If one of these compounds remains, it is then advisable to adjust the amount of chlorine in order to consume the residual product. At the end of the reaction, the monochlorobenzene is distilled off by placing the reactor under gradually increasing vacuum through a distillation column. After removal of the solvent, the 2,6-dichloro-para-trifluoromethylaniline is cooled to 60C before emptying the reactor to the storage tank.

References:

WO2004/37766,2004,A2 Location in patent:Page 4

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