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With tetrabutoxytitanium; 4-methylisopropylbenzene; 4-methoxy-phenol; at 89 - 102℃; under 30.003 Torr;
100.0 g (purity: 93.7%, 0.64 mol in terms of purity) of 14 BDMGE, 150.1 g (0.96 mol) of tetrahydrofurfuryl acrylate were placed in a 500 ml four-necked flask equipped with a distillation apparatus, a thermometer, , P-cymene (200.0 g) and MEHQ (0.03 g) were added to prepare a raw material mixture solution (total 450.1 g). The moisture content of the raw material mixture liquid was measured with a Karl Fischer moisture meter to be 547 ppm, and the total amount of moisture contained was 0.25 g (0.014 mol). TBT (4.4 g, 0.013 mol) was added to the above raw material mixture, and the temperature was raised with stirring while reducing the pressure to 40 hPa, while p-cymene and tetrahydrofurfuryl alcohol to be produced were distilled out of the reaction system , And the transesterification reaction was carried out at a reaction solution temperature of 89 to 102 C. The temperature of the distillation gas was 69 to 78 C. Finally, 196.6 g of the fraction was withdrawn in 11 hours to terminate the reaction, and 252.2 g of a reaction solution containing 4 HBAGE (43.2 wt%) was obtained. The purity-converted quantitative yield of 4HBAGE is 84.9%, and the molar ratio of the total amount of moisture in this reaction system is 1.1 times the TBT used. 140.0 g of water and 100.0 g of additional p-cymene were added to the above reaction solution, heated to 60 C. under normal pressure and stirring, and heated and hydrolyzed at 60 C. for 1 hour as it was. The reaction solution was cooled and suction filtered using a filter equipped with Celite to remove insoluble catalyst. The filtrate was separated into an organic layer and an aqueous layer. The organic layer containing 4 HBAGE was concentrated under reduced pressure using a rotary evaporator to obtain 124.0 g of 4 HBAGE crude product (purity 88.2%). The purity-converted quantitative yield of 4 HBAGE was 85.2%, and the titanium content derived from TBT used as a catalyst was 2 ppm or less. 50.0 g of the above 4 HBAGE crude product (124.0 g) was fractionated, 0.08 g of CBC was added thereto, and purification was carried out by simple distillation under reduced pressure. As a result, high purity 4 HBAGE (purity 96.6%) 37.7 g. The purity-converted quantitative yield of 4 HBAGE is 70.4% in terms of the consistent yield from the transesterification reaction. Conditions at the time of fractional distillation were 0.4 to 0.5 hPa for the degree of vacuum, 97 to 112 C. for the bottom liquid temperature, 89 to 91 C. for the distillation gas temperature and 30 to 30 hours for the distillation time Min. No polymer was observed in the distillation residue and in the distillation system.
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