M-Xylene → Methyl isobutyrate

Beteiligte Stoffe

Reaktionsschritte

A stainless steel-made tubular reactor to be used as a hydrogenation reactor having an inside diameter of 15 mm and a length of 300 mm was packed inside with 10 g of copper-chromite as the catalyst roughly uniformized in particle size of 10 to 20 mesh (produced by Nissan Girdler Catalyst Co.,Ltd. under the trade name: G-99C in the form of pellets). Subsequently, a catalyst reduction was carried out at 150 to 200° C. by passing through the reactor, hydrogen gas diluted with nitrogen to 0.5 to 5% by volume by the conventional method with sufficient care not to form a hot spot. Thereafter, the feed gas to the reactor was switched to pure hydrogen at a pressure of 70 kg/cm2G, a purge gas SV of 500 hr-1 and a catalyst bed temperature of 230° C. Then, the tubular reactor was charged at an upper portion thereof with a starting material for reaction consisting of a solution of 30 parts by weight of 2-methyl-γ-butyrolactone which had been obtained in Example 3 in 70 parts by weight of m-xylene at a rate of 3.3 g per hour. The effluent through a lower portion thereof was cooled and degasified to collect the reaction product. After the lapse of 5 hours from the start of the reaction, the reaction product was collected for one hour and analyzed by gas chromatography. As a result, the objective 3-methyltetrahydrofuran was obtained in a yield of 90.1% in a conversion efficiency of 2-methyl-γ-butyro-lactone of 100% in a yield of 0.5% methyl isobutyrate, while methanol was not detected in the reaction product throughout the reaction period.

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