文章摘要
[(4-(N,N-二甲氨基)苯基]二叔丁基磷的合成工艺
Synthesis of [(4-Dimethylaminophenyl)]di(tert-butyl)phosphine
投稿时间:2018-01-24  修订日期:2018-04-09
DOI:
中文关键词: [(4-(N,N-二甲氨基)苯基]二叔丁基磷,[(4-(N,N-二甲氨基)苯基]二氯化磷,N,N-二甲基苯胺,催化,精细化工中间体
英文关键词: [(4-Dimethylaminophenyl)]di(tert-butyl)phosphine, Dichloro-4-(N,N-dimethylamino)phenylphosphane, N,N-dimethylaniline, catalyst, fine chemical intermediates
基金项目:
作者单位E-mail
陈辉 河南省科学院化学研究所有限公司 hchen@kingorgchem.com 
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中文摘要:
      以 N,N-二甲基苯胺为原料,经与三氯化磷和吡啶反应生成[(4-(N,N-二甲氨基)苯基]二氯化磷 (I),然后在碘化亚铜和溴化锂的催化作用下与叔丁基氯化镁反应得到[(4-(N,N-二甲氨基)苯基]二叔丁基磷 (Ⅱ) ,采用31PNMR、1HNMR和HRMS 对目标化合物进行结构表征,通过考察各步的反应条件,得出最佳的工艺条件:n (N,N-二甲基苯胺) : n (三氯化磷) : n (吡啶) = 1 : 3 : 3,110 ℃反应 24 h,[(4-(N,N-二甲氨基)苯基]二氯化磷的收率为85.3%;n(化合物Ⅰ): n (碘化亚铜) : n (溴化锂) : n (叔丁基氯化镁) = 1 : 0.1 : 0.2 : 3,40 ℃反应 12 h,[(4-(N,N-二甲氨基)苯基]二叔丁基磷收率可达83.4%。
英文摘要:
      [(4-Dimethylaminophenyl)]di(tert-butyl)phosphine was prepared in two steps. Dichloro-4-(N,N-dimethylamino)phenylphosphane was firstly synthesized from N,N-dimethylaniline and PCl3 as starting materials. And the title compound was funished by coupling reaction of dichloro-4-(N,N-dimethylamino)phenylphosphane and tert-butylmagnesium chloride. Structure characterization of the intermediates was conducted by methods of 31PNMR、1HNMR and HRMS. The optimum reaction conditions were determined as follows: n (N,N-dimethylaniline) : n (PCl3) : n (pyridine) = 1 : 3 : 3,the reaction temperature and time was 110 ℃ and 24 h, the yield of Ⅰ was 85.3%. In the coupling step, n(Ⅰ): n (CuI) : n (LiBr) : n (t-BuMgCl) = 1 : 0.1 : 0.2 : 3,[(4-dimethylaminophenyl)]di(tert-butyl)phosphine was got in yield of 83.4% at 40 ℃ for 12 h.
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