反应详情

To a mixture of 4,367 kilograms (32.75 moles) of aluminum chloride and 8.8 liters of dichloromethane at 0° C. is added gradually a solution of 3,267 kilograms of 1,4-bis(2,2,2-trifluoroethoxy)benzene and 1.399 kilograms (13.7 moles) of acetic anhydride in 1.3 liters of dichloromethane. The reaction temperature is maintained at 5° to 10° C. while stirring the mixture for about 16 hours. The reaction mixture is then heated to its reflux temperature and maintained under reflux for 4 hours. The reaction mixture is then acidified with 8.76 kilograms of 10 percent hydrochloric acid. Ice is added to the mixture to maintain the temperature below 20° C. The organic layer is separated and the aqueous layers are extracted several times with dichloromethane. The organic layers are dried, then evaporated to provide a residue which is triturated with hexane to provide a yellow solid product. Two crops of product are obtained providing a total yield of 3.088 kilograms of 2,5-bis(2,2,2-trifluoroethoxy)acetophenone, m.p. 84° to 88° C., yield 82 percent.

1. temperatureThe reaction temperature is maintained at 5° to 10° C.
2. temperatureThe reaction mixture is then heated to its
3. temperaturereflux temperature
4. temperaturemaintained
5. temperatureunder reflux for 4 hours
6. additionIce is added to the mixture
7. temperatureto maintain the temperature below 20° C
8. customThe organic layer is separated
9. extractionthe aqueous layers are extracted several times with dichloromethane
10. customThe organic layers are dried
11. customevaporated
12. customto provide a residue which
13. customis triturated with hexane
14. customto provide a yellow solid product
15. customTwo crops of product are obtained