双(3,5-二甲基苯基)膦的合成

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.

Preparation of bis(3,5-dimethylphenyl)phosphine

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 bis(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.