反应详情

The step was performed according to the method described in U.S. Pat. No. 4,272,284. Xylylene dibromide (160 g, 606 mmol) and compound (88.52 g, 606 mmol) obtained in step A were dissolved in N-methylpyrrolidone (550 ml). While maintaining the reaction mixture at 50° C.-60° C., triethylamine (190 ml, 1.36 mol) was gradually added dropwise using infundibulum with stirring and, after the completion of the dropwise addition, the reaction mixture was stood overnight at room temperature. A 5% aqueous citric acid solution (700 ml) was added to the reaction mixture, and the precipitated solid was collected by filtration, washed with water and dried under reduced pressure to give the title compound (126 g, yield 84%) as a crude pale-pink solid.

1. temperatureWhile maintaining the reaction mixture at 50° C.-60° C.
2. additionafter the completion of the dropwise addition
3. filtrationthe precipitated solid was collected by filtration
4. washwashed with water
5. customdried under reduced pressure