反应详情

温度

0 °C

To the solution of 440 g of 1,2-dihydroxybenzene dissolved in 1L of ethylene dichloride was added 1036 g of trichloroacetaldehyde monohydrate and then the reaction solution was cooled down to 0° C. 102 g of triethylamine was slowly added dropwise thereto. The reaction solution was warmed to normal temperature, stirred for about 20 minutes, heated to 50° C. and then stirred for further 3 hours while maintaining the same temperature. After the reaction is completed, the reaction mixture was distilled under reduced pressure to remove ethylene dichloride. The residue was dissolved in 4L of ethylacetate, washed successively with 2400 ml of 0.5N-aqueous hydrochloric acid solution and 2L of saturated saline solution, dried over anhydrous magnesium sulfate and then distilled under reduced pressure to remove the solvent to obtain 540 g of the title compound.

1. temperatureThe reaction solution was warmed to normal temperature
2. temperatureheated to 50° C.
3. stirringstirred for further 3 hours
4. temperaturewhile maintaining the same temperature
5. distillationthe reaction mixture was distilled under reduced pressure
6. customto remove ethylene dichloride
7. dissolutionThe residue was dissolved in 4L of ethylacetate
8. washwashed successively with 2400 ml of 0.5N-aqueous hydrochloric acid solution and 2L of saturated saline solution
9. dry with materialdried over anhydrous magnesium sulfate
10. distillationdistilled under reduced pressure
11. customto remove the solvent