反应详情

In a 3-L flask equipped with a stirrer, a thermometer and a dropping funnel, 110 g (522.39 mmol) of anhydrous trimellitic chloride (4-chlorocarbonylphthalic anhydride) and 770 g of 1,4-dioxane were placed and were stirred at room temperature in an atmosphere of a nitrogen gas. To the resulting mixture, a mixture of 92.70 g (497.52 mmol) of 1-dodecanol, 41.32 g (522.39 mmol) of pyridine and 370 g of 1,4-dioxane was added dropwise over 1 hour. The mixture was stirred at room temperature for further 5 hours, followed by dropwise addition of 570 g of pure water over 30 minutes. Pyridine hydrochloride separated in a reaction system was then dissolved, and a crystal of target 4-dodecyloxycarbonylphthalic anhydride separated out. The resulting mixture was stirred for further 1 hour, the precipitate was separated by filtration and was rinsed with pure water, was then dried at 50° C. under reduced pressure and thereby yielded 145.26 g (402.99 mmol) of 4-dodecyloxycarbonylphthalic anhydride as a white powder. The yield was 80.1% on the basis of 1-dodecanol and 77.1% on the basis of anhydrous trimellitic chloride.

1. customIn a 3-L flask equipped with a stirrer
2. additionwas added dropwise over 1 hour
3. stirringThe mixture was stirred at room temperature for further 5 hours
4. customPyridine hydrochloride separated in a reaction system
5. dissolutionwas then dissolved
6. customa crystal of target 4-dodecyloxycarbonylphthalic anhydride separated out
7. stirringThe resulting mixture was stirred for further 1 hour
8. customthe precipitate was separated by filtration
9. washwas rinsed with pure water
10. customwas then dried at 50° C. under reduced pressure