The best process conditions of the synthesis of 3,3- dimethyl-1-butene(new hexene) were discussed. With tertiary butyl alcohol and hydrochloric acid as raw materials, concentrated sulfuric acid as catalyst for synthesis of chlorinated tertiary butane, the influence of reaction temperature and reaction time on the yield were discussed.Using compression method with anhydrous AlCl3 as catalyst, chlorinated new hexane (2, 2 - dimethyl butane) was synthesized with chlorinated tertiary butane and ethylene as raw materials. The suitable addition reaction conditions were determined, with N - methyl pyrrolidone as solvent, adopting the method of reaction distillation，neohexene was prepared after hydrogen chloride was removed from chlorinated new hexane.The obtained best process conditions were that in the synthesis of chlorinated tertiary butane,the optimum reaction temperature was 20 ℃, and the best reaction time was 60 min; in the synthesis of chlorinated new hexane ,the optimum reaction pressure was 0.75 MPa, the best reaction temperature was 45℃; N - methyl pyrrolidone was the best solvent for the preparation of nehexene by dehydrochlorination.