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ChemicalBook CAS DataBase List 2,3-Dimethyl-1-butene

2,3-Dimethyl-1-butene synthesis

10synthesis methods
187737-37-7 Synthesis
propene

187737-37-7
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Yield:563-78-0 90%

Reaction Conditions:

with diethyl aluminiumcholoride;trioctyl phosphite in toluene at -10; under 1500.15 Torr; for 5 h;Inert atmosphere;Autoclave;Reagent/catalyst;Temperature;

Steps:

1-40 Example 33
(1) Catalyst preparationThe activated 10 g molecular sieve ZSM-5 contains 1.56 g of nickel nitrate and 1.55 g.Impregnating a solution of cobalt nitrate in nitric acid, filtering, washing with water, roasting, reduction,5% Ni-5% Co/ZSM-5 catalyst was obtained by vacuum distillation;(2) Feeding7 g of 5% Ni-5% Co/ZSM-5 catalyst was added to 140 g of toluene solvent.Add 7g of trioctyl phosphite, mix and mix in a low temperature tank to cool,0.35 g of diethylaluminum chloride was added under nitrogen protection.The autoclave was evacuated to -0.01 MPa.Negative pressure presses the material into the autoclave;(3) Passing propylene gasPassing a cooling medium to a temperature of -10 ° C, and intermittently introducing 84 g of propylene gas into the autoclave at a pressure of 0.2 Mpa;(4) ReactionAfter reacting for 5 hours, the experiment was terminated and the reaction was quenched;(5) FilteringThe reaction solution is recovered by filtration;(6) RectificationDistillation separation gave 68.88 g of 2,3-dimethyl-1-butene in a yield of 90% and a selectivity of 91.5%.

References:

Shandong Xinhecheng Pharmaceutical Co., Ltd.;Fang Wanjun;Ma Xiao;Du Rongqiang;Zhong Juanjuan;Wang Ziming;Li Congcong;Dong Fengchan;Fan Guotao CN110002936, 2019, A Location in patent:Paragraph 0026-0065

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