丙酮酸钠合成工艺研究
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摘要
以空气为氧化剂,9-氮杂双环[3.3.1]壬烷-N-氧基自由基为催化剂,亚硝酸钠为助催化剂,1atm空气催化氧化合成丙酮酸乙酯。丙酮酸乙酯经水解、碳酸氢钠中和制得丙酮酸钠。考察了各种因素对反应的影响,确定了最佳的反应条件。在此条件下,丙酮酸乙酯收率为92%,丙酮酸钠的收率为93%。
Ethyl pyruvate was synthesized by air catalytic oxidation,1 atm air as oxidant,9-azabicyclo[3.3.1]decane-N-oxyl radical as catalyst,sodium nitrite as cocatalyst.Ethyl pyruvate ws hydrolyzed and neutralized by sodium bicarbonate to obtain sodium pyruvate.The effects of several factors on the reaction were investigated and the optimal reaction conditions were determined.The yield of ethyl pyruvate can reach 92%,and the yield of sodium pyruvate can reach 93%.
Ethyl pyruvate was synthesized by air catalytic oxidation,1 atm air as oxidant,9-azabicyclo[3.3.1]decane-N-oxyl radical as catalyst,sodium nitrite as cocatalyst.Ethyl pyruvate ws hydrolyzed and neutralized by sodium bicarbonate to obtain sodium pyruvate.The effects of several factors on the reaction were investigated and the optimal reaction conditions were determined.The yield of ethyl pyruvate can reach 92%,and the yield of sodium pyruvate can reach 93%.
引文
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[7]Markus B Lauber,Shannon S Stahl.Efficient aerobic oxidation of secondary alcohols at ambient temperature with an ABNO/Nox catalyst system[J].ACS Catal,2013,3,2612-2616.
[2]张庆勇.丙酮酸剂丙酮酸钠制备[J].化学试剂,1997,19(6):375-336.
[3]Bobbitt J M,Brückner C,Merbouh N.For a recent comprehensive review of nitroxyl-mediated and catalyzed methods for alcohol oxidation[J].Org React,2009,74,106-132.
[4]Liu R,Liang X,Dong C,et al.For catalytic aerobic alcohol oxidation methods that employ nitrate/nitrite cocatalysts with TEM-PO[J].J Am Chem Soc,2004,126,4112-4113.
[5]Ben-Daniel R,Alsters P,Neumann R.For examples of catalytic aerobic alcohol oxidation methods that employ TEMPO in combination with cocatalysts other than nitrate or nitrite[J].J Org Chem,2001,66,8650-8653.
[6]Kuang Y,Islam N M,Nabae Y,et al.Selective aerobic oxidation of benzylic alcohols catalyzed by carbon-based catalysts:a nonmetallic oxidation system[J].Angew Chem Int Ed,2010,49,436-440.
[7]Markus B Lauber,Shannon S Stahl.Efficient aerobic oxidation of secondary alcohols at ambient temperature with an ABNO/Nox catalyst system[J].ACS Catal,2013,3,2612-2616.