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[目的]旨在优化出一条适合工业化生产2,2-二氟苯并[1,3]间二氧杂环戊烯-4-甲醛的工艺路线。[方法]以邻甲酚为起始原料,经“一锅煮”得到3-甲基苯邻二酚,再经醚化、氯化、氟交换和水解5步反应得2,2-二氟苯并[1,3]间二氧杂环戊烯-4-甲醛。[结果]反应总收率35.1%,含量99.5%(GC),产物与中间体经1H NMR、MS等进行了表征。[结论]提高了收率,简化了操作,适合工业化生产。
[Objective] The aim was to optimize a suitable process for the industrial production of 2,2-difluorobenzo [1,3] dioxole-4-carbaldehyde. [Method] With o-cresol as the starting material, 3-methylbenzene phthalic acid was obtained by “one-pot cooking”, then reacted with etherification, chlorination, fluorine exchange and hydrolysis in 5 steps to obtain 2,2- Benzo [1, 3] dioxole-4-carbaldehyde. [Result] The total yield of the reaction was 35.1% and the content was 99.5% (GC). The products and intermediates were characterized by 1H NMR, MS and so on. [Conclusion] The yield was raised, the operation was simplified, and it was suitable for industrial production.