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ChemicalBook CAS DataBase List Ethyl chlorooxoacetate

Ethyl chlorooxoacetate synthesis

10synthesis methods
-

Yield:4755-77-5 127 g

Reaction Conditions:

with dichloro sulfoxide in 5,5-dimethyl-1,3-cyclohexadiene at 60; for 4 h;Reagent/catalyst;Solvent;

Steps:

4-5

133 grams of the above-mentioned crude ethyl oxalate monopotassium salt (determined by liquid chromatography that the molar weight of ethyl oxalate monopotassium salt is 952 mmol) was suspended in 150 milliliters of xylene, and 125 grams of thionyl chloride (1.05 gram) was added dropwise with stirring. mol), the internal temperature was 60 °C for 4 hours. According to the requirements of environmental protection, secondary water absorption (possible trace hydrogen chloride) and primary liquid alkali absorption (sulfur dioxide) are carried out. The product is distilled under reduced pressure, and fractions at 133-135° C. are collected to obtain 127 g of oxalyl chloride monoethyl ester product, the content detected by GC is 99.6%, and the total yield of two steps is 93%.

References:

CN114805065,2022,A Location in patent:Paragraph 0059; 0061; 0062; 0064

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