Ionic liquids （ILs） based on 1,3-dialkylimidazolium and tetraalkylammonium cations were employed as a series of efficient, environmentally benign phase-transfer catalysts （PTCs） for the base-promoted monoalkylatio...Ionic liquids （ILs） based on 1,3-dialkylimidazolium and tetraalkylammonium cations were employed as a series of efficient, environmentally benign phase-transfer catalysts （PTCs） for the base-promoted monoalkylation of diethyl malonate. The influence of various heterogeneous bases on yields was studied. Good yields and high selectivity were obtained. Solvent-free, mild reaction condition, short reaction time, and easy purification were the merits of this method. The catalytic system （IL-hase） could also be recycled after the extraction of products with ether.展开更多
Diethyl malonate being an initial raw material, processed with chlorination-replacement-desalination-vacuum rectification, is used to produce carbonyl diethyl malonate. An experiment for optimization determines that t...Diethyl malonate being an initial raw material, processed with chlorination-replacement-desalination-vacuum rectification, is used to produce carbonyl diethyl malonate. An experiment for optimization determines that the best reaction condition was： （1 reaction for 7 h at 10 ℃ with mole-ratio being 2.4 ＂ 1 between chloride and raw material （diethyl malonate）; （2 reaction for 4.5 h at 118 ℃ with mole-ratio being 1.2 ： 1 between the anhydrous sodium acetate and intermediate I. The final product carbonyl diethyl rnalonate recovery ratio reaches up to as high as 79.12% with a purity of 96.4%, which meets the market requirement. This synthesis technique has the advantages of simple process, moderate reaction conditions, high yield and low cost, being suitable for industrial scale production.展开更多
The title complex {CpEu CH(COOC 2H 5) 2 μ CH(COOC 2H 5) 2 } 2 crystallizes in the triclinic system, space group P1 with unit cell constants a=9.108(1), b=11.580(2), c=11.705(2) , α=70.42(1)...The title complex {CpEu CH(COOC 2H 5) 2 μ CH(COOC 2H 5) 2 } 2 crystallizes in the triclinic system, space group P1 with unit cell constants a=9.108(1), b=11.580(2), c=11.705(2) , α=70.42(1)°, β=73.83(1)°, γ=78.60(1)°, D c =1.602 g/cm 3 , M r=1070.76, V=1109.7(3) 3, Z=1, μ (Mo Kα )=28 66 cm 1 and F(000)=536, T=296K, R=0.028, R w =0.037. The geometry around the Eu ion can be described as a pentagonal bipyramid.展开更多
文摘Ionic liquids （ILs） based on 1,3-dialkylimidazolium and tetraalkylammonium cations were employed as a series of efficient, environmentally benign phase-transfer catalysts （PTCs） for the base-promoted monoalkylation of diethyl malonate. The influence of various heterogeneous bases on yields was studied. Good yields and high selectivity were obtained. Solvent-free, mild reaction condition, short reaction time, and easy purification were the merits of this method. The catalytic system （IL-hase） could also be recycled after the extraction of products with ether.
基金Supported by the Innovation Fund for Technology Based Firms(10C26224212340)
文摘Diethyl malonate being an initial raw material, processed with chlorination-replacement-desalination-vacuum rectification, is used to produce carbonyl diethyl malonate. An experiment for optimization determines that the best reaction condition was： （1 reaction for 7 h at 10 ℃ with mole-ratio being 2.4 ＂ 1 between chloride and raw material （diethyl malonate）; （2 reaction for 4.5 h at 118 ℃ with mole-ratio being 1.2 ： 1 between the anhydrous sodium acetate and intermediate I. The final product carbonyl diethyl rnalonate recovery ratio reaches up to as high as 79.12% with a purity of 96.4%, which meets the market requirement. This synthesis technique has the advantages of simple process, moderate reaction conditions, high yield and low cost, being suitable for industrial scale production.
文摘The title complex {CpEu CH(COOC 2H 5) 2 μ CH(COOC 2H 5) 2 } 2 crystallizes in the triclinic system, space group P1 with unit cell constants a=9.108(1), b=11.580(2), c=11.705(2) , α=70.42(1)°, β=73.83(1)°, γ=78.60(1)°, D c =1.602 g/cm 3 , M r=1070.76, V=1109.7(3) 3, Z=1, μ (Mo Kα )=28 66 cm 1 and F(000)=536, T=296K, R=0.028, R w =0.037. The geometry around the Eu ion can be described as a pentagonal bipyramid.
