双(3,5-二甲基苯基)膦的合成

Preparation of bis(3,5-dimethylphenyl)phosphine

为了推动在国内尚无商业化产品的双(3,5-二甲基苯基)膦在不对称催化合成精异丙甲草胺中应用,对双(3,5-二甲基苯基)膦的合成工艺进行了研究.以双(3,5-二甲基苯基)氧膦为原料,通过二异丁基氢化铝还原得到双(3,5-二甲基苯基)膦,最佳条件为:双(3,5-二甲基苯基)氧膦与二异丁基氢化铝摩尔比为1∶3,溶剂为四氢呋喃,反应温度65℃,反应时间1 h,产率为89%.实验结果表明:该方法操作简单,副反应少且容易控制.

Bis（3,5-dimethyl phenyl）phosphine is an effective ligand for asymmetric synthesis of S-metolachlor and there is no commercial product in domestic at present. In order to promote the development of asymmetric synthesis process of S-metolachlor, the synthetic process was studied in this paper. With bis （3,5-dimethyl phenyl） phosphine oxide as raw material, bis （3,5-dimethyl phenyl）phosphine was synthesized by deoxidization through diisobutyl aluminium hydride, and the optimal conditions were the ration of his （3,5-dimethyl phenyl） phosphine oxide to diisobutyl aluminum hydridemole of 1 ： 3, reaction temperature of 65 ℃, reaction time of 1 h, and the production rate of 89% . The results show that this method is simple, and easy to control with less side reactions.