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S3 S3)Synthesis of N-(o-methoxyphenoxyethyl)-phthalimide:
31g of intermediate prepared by S2)27.6 g of phthalimide potassium salt was dissolved in 100 g of DMF,After refluxing at 170 ° C for 3 h, after TLC analysis without raw materials,50 ml of DMF was distilled off under reduced pressure, and 100 g of methanol was added to disperse.Cool down and filter, wash once,Recrystallization from 95% ethanol to give intermediate41.2g,HPLC content is not less than 97%,The yield was 86.4%.
With tetrabutylammomium bromide at 180 - 185℃;
2
Example 2: Preparation of Phthalimide derivative of l-(2-Chloro- ethoxy)-2-methoxy-benzene150 kg of pure l-(2-Chloro ethoxy)-2-methoxy benzene obtained according to the procedure described in Example 1, 195 kg of Potassium Phthalimide and 7.5 kg of tetrabutyl ammonium bromide were charged in a reactor and heated to about 180 °C and stirred for about 3 hours at about 180 °C to 185 °C. The reaction mixture was transferred in to a container having 1650 L of water and the precipitated solid was filtered. The wet material (300 kg) was charged into a reactor containing 300 L of methanol and heated to reflux. The contents were stirred at reflux for about 1 hour. The reaction mixture was cooled to ambient temperature and filtered the solid .The wet solid was dried at 60-80 0C to obtain 2-10 kg of the title compound.
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