三氯吡啶酚及其钠盐的合成

Synthesis of 3,5,6-Trichloropyridin-2-ol and Its Salt

用一种简单的方法合成了 3,5 ,6 三氯吡啶 2 酚及其钠盐。三氯乙酰氯和丙烯腈在催化剂CD 存在下 ,以硝基苯作溶剂 ,回流下连续完成加成与环化 ,再芳构化 ,得 3,5 ,6 三氯吡啶 2 酚或其钠盐。三氯乙酰氯 91 0 g、丙烯腈 34 5 g、硝基苯 2 0 0mL及催化剂CD1 4 g加热回流约 4h至 14 5℃ ,恒温 5h。得三氯吡啶酚钠 77 8g(收率 70 6 % )或得三氯吡啶酚 71 5 g(收率72 1% )。w(三氯吡啶酚 ) =95 8%。

A simple process for synthesis of 3,5,6 trichloropyridin 2 ol and its salt was developed.Trichloroacetyl chloride reacted with acrylonitrile under reflux in the presence of a catalyst and a solvent to give 3,3,5,6 tetrachloro dihydropyridin 2 one, which was aromatized to 3,5,6 trichloropyridin 2 ol sodium,and acidized to 3,5,6 trichloropyridin 2 ol.Thus,91 0 g trichloroacetyl chloride and 34 5 g acrylonitrile were refluxed with 1 4 g catalyst C D in 200 mL nitrobenzene at 145 ℃ for 4 h and maintained for 5 h to produce 77 8 g 3,5,6 trichloropyridin 2 ol sodium or 71 5 g 3,5,6 trichloropyridin 2 ol (in >70% yield and 95.8% purity).