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报道了无酸和重金属盐的催化乙炔双羰化反应的钯催化体系(催化剂组成为Pd Cl2/KI).正交实验表明空气的初始分压和助剂KI的用量在乙炔双羰化反应中起着重要的作用.在相同的实验条件下,发现催化体系为Pd Cl2/HCl/Cu Cl2和Pd Cl2/H_2SO4/Fe Cl3时,顺、反丁烯二酸二甲酯的总收率分别为15.3%和21.8%,而用Pd Cl2/KI时总收率达到了81.9%.在最优反应条件下,即Pd Cl20.056 mmol,KI 0.677 mmol,总压5.3 MPa,70℃反应3 h,顺、反丁烯二酸二甲酯的总收率为91.0%.
Reported the palladium-catalyzed acetylene dicarbonylation reaction catalyzed by acid and heavy metal salts (catalyst composition of PdCl2 / KI) .The orthogonal experiment showed that the initial partial pressure of air and the amount of KI additive in the acetylene bicarbonylation reaction Plays an important role in the same experimental conditions, the catalyst system was found to PdCl2 / HCl / Cu Cl2 and Pd Cl2 / H_2SO4 / Fe Cl3, cis, the total yield of dimethyl fumarate were 15.3% and 21.8%, respectively, while the total yield reached 81.9% with PdCl 2 / KI.The optimal reaction conditions were as follows: PdCl 20.056 mmol, KI 0.677 mmol, total pressure 5.3 MPa, reaction at 70 ℃ for 3 h, The overall yield of dimethyl fumarate was 91.0%.