Oxygen → Dibutyl Oxalate

関与物質

反応手順

The following materials were charged to the autoclave: a solution of 0.19 g. lithium iodide (1.41 mmoles), 2.34 g. triethylamine (23.0 mmoles), 6.96 g. triethylammonium sulfate (23.0 mmoles), 50 ml n-butanol (0.546 mole), and 61.7 g. of a mixture of 70.6 weight percent cyclohexanone di-n-butyl ketal (0.191 mole), 8.4 weight percent cyclohexanone, and 19.6 weight percent n-butanol (0.163 mole). The charged solids were 0.25 g. palladium (II) iodide (0.69 mmole) and 3.70 g. anhydrous copper (II) sulfate (23.0 mmoles). The reaction temperature was 100° C. The initial pressure at reaction temperature was 1500 psi. 100 psi oxygen was charged followed by 200 psi CO. An exotherm and pressure drop were noted. The oxygen/CO cycle was repeated seven more times. A total of 1870 psi pressure drop was observed during a reaction time of approximately 4.1 hours. The total pressure varied between 1500 and 2190 psi. According to gas-liquid chromatographic analysis, cyclohexanone and n-butanol were present while all of the ketal was consumed. Di-n-butyl oxalate (27.3 g.; 98 percent; 0.132 mole) was isolated by distillation and identified by spectroscopic analysis. Di-n-butyl carbonate was detected in the distillate.

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