[(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．