2,2-二氟苯并1,3间二氧杂环戊烯-4-甲醛的合成新工艺

摘要

研究了2,2-二氟苯并[1,3]间二氧杂环戊烯-4-甲醛的合成反应条件。以邻甲苯酚为原料,经＂一锅煮＂得到中间体3-甲基苯邻二酚,再经醚化、氯化、氟交换和水解5步反应得到2,2-二氟苯并[1,3]间二氧杂环戊烯-4-甲醛,在优化的反应条件下,反应总收率为33.2%,目标产物含量99.7%,用IR、1H NMR表征了其结构。%2,2-difluoro-1,3-benzodioxol-4-aldehyde was the key intermediate of fungicide fludioxonil.The synthetic process of 2,2-difluoro-1;3-benzodioxol-4-aldehyde was studied in order to improve the yield and the purity of the product.The title compound was prepared from o-cresol as the raw material via five steps including one pot synthesis of 3-methyl-1,2-benzene-diol,and then etherification,chlorination,fluorination,and hydrolysis.Under the optimal condition,the total yield was 33.2%,and the purity was 99.7%.The structure of the resulting product was confirmed by IR、1^H NMR.