Example 12
Synthesis of Compound A-2-3
5.4 g (25 mmol) of 1-(acryloyloxy)-3-(methacryloyloxy)-2-propanol, manufactured by Tokyo Chemical Industry Co., Ltd. was added to 100 mL of dehydrated dichloromethane. After replacing the inside of the flask with argon gas, 3.6 g (36 mmol) of triethylamine was added.
After cooling the mixture to about −10 degrees C., 2.4 g (30 mmol) of acetic acid chloride was slowly dripped in such a manner that the system temperature became −10 to −5 degrees C. followed by two-hour stirring at room temperature. Moreover, after precipitates were removed by filtration, the filtrate was rinsed with water, an aqueous solution of saturated sodium hydrogen carbonate, and an aqueous solution of saturated sodium chloride.
Thereafter, subsequent to drying with sodium sulfate, the resultant was condensed under a reduced pressure to obtain yellow oily matter. Furthermore, 200 g of Wakogel C300 (manufactured by Wako Pure Chemical Industries, Ltd.) was loaded, and the yellow oily matter was purified by column chromatography using hexane and ethyl acetate as an eluent to obtain 1.8 g (yield: about 28 percent) of colorless oily matter of the compound represented by the chemical formula illustrated in Table 1-2. The purity was 99.1 percent by mass.