2,2'-亚甲基双(4,6-二叔丁基苯基)磷酰氯的合成与表征

Synthesis and Characterization of 2,2′-Methylene-bis(4,6-di-tert-butylphenyl) Phosphate Chloride

以2,2'-亚甲基双(4,6-二叔丁基苯)酚为原料,三乙胺作为溶剂与缚酸剂,合成聚丙烯成核剂2,2'-亚甲基双(4,6-二叔丁基苯基)磷酰钠(NA-11)的中间体2,2'-亚甲基双(4,6-二叔丁基苯基)磷酰氯。主要讨论了反应条件、三氯氧磷(POCl3)的滴加温度、反应温度、以及反应时间对收率的影响。结果表明:当POCl3滴加温度为5℃、反应温度为40℃、反应2 h下收率为85.16%,产品质量较好。重结晶溶剂选择乙腈。对产物进行了IR、TGA、1H NMR与MS表征。结果表明:产物结构与2,2'-亚甲基双(4,6-二叔丁基苯基)磷酰氯相一致。

2,2＇-methylene-bis （4,6-di-tert-butylphenyl） phosphate chloride, which was the intermediate of sodium of 2,2＇- methylene-his （ 4,6-di-tert-butylphenyl ） phosphate （ NA-11 ） , was prepared with 2, 2＇-methylene-his （ 4, 6-di-tert- butylphenol） as raw material and triethylamine as solvent and acid binding agent. The influences of the reaction conditions including the dropping temperature of POCI3 ,the reacting temperature and the reacting time on the yield of the product were discussed. The result showed when the dropping temperature of POC13 was 5 ~C , the reacting temperature was 40 ~C , and the reacting time was 2 h,the yield of the product with good quality was 85.16 %. The acetonitrile was selected as reerystallization solvent. The structure of the product was characterized by IR, TGA,~H NMR and MS methods. The result indicated that the structure of the product was consistent with that of 2,2＇-methylene-bis （4,6-di-tert-butylphenyl） phosphate chloride.