Chlorosilyl dichloroboryl ethane, Cl[(CH3)(2)]Si-CH(CH3)-BCl2 (CSDE), is an important precursor used to prepare Si/B/C/(N) ceramics, which can be synthesized by the hydroboration reaction. An optimized synthesis route to prepare CSDE was found by examining the reaction conditions, including the ratio of reactants and reaction time through an orthogonal experiment. In addition, an unknown by-product was also studied during the orthogonal experiment By analyzing and calculating the results of (HNMR)-H-1, (CNMR)-C-13, and B-11 NMR, the following conditions were found to be optimal for this reaction: TESH(Et3SiH):TCB(BCl3):CDVS (CH2=CH-Si(CH3)(2)Cl) = 1.025:1.2:1; reaction time: 20 min