반응 #47133

반응 방정식

benzoyl chloride

N-hydroxyphthalimide

pyridine

1,4-dioxane

→

N-benzoyloxyphthalimide

용매

water

반응 조건

후처리

1. 1
   기타In a 3-L flask equipped with a stirrer
2. 2
   workup.STIRRINGthe resulting mixture was stirred at room temperature for further 2 hours
3. 3
   workup.DISSOLUTIONto dissolve
4. 4
   기타by-produced salts

실험 절차

In a 3-L flask equipped with a stirrer and thermometer, 100 g (613 mmol) of N-hydroxyphthalimide, 53.3 g (674 mmol) of pyridine and 1100 g of 1,4-dioxane were placed and were stirred at room temperature. To the resulting mixture, 94.8 g (674 mmol) of benzoyl chloride was added dropwise over 1 hour, and the resulting mixture was stirred at room temperature for further 2 hours. Subsequently, 1100 g of pure water was added dropwise over 30 minutes to dissolve by-produced salts and thereby yielded a crystal of the target N-benzoyloxyphthalimide. The mixture was stirred and aged for further 1 hour, the crystal was filtrated using a Nutsche, was rinsed with an appropriate amount of water, was dried at 60° C. under a reduced pressure and thereby yielded 162 g (604 mmol) of N-benzoyloxyphthalimide in a yield of 98.6% on the basis of N-hydroxyphthalimide.

출처