Sodium Bicarbonate → Butanediol glycidyl ether

Participants

Reaction Steps

A 1-L four-necked separable flask was charged with 5.0 g of sodium hydrogen sulfate and 140 g of pure water and then provided with a stirrer, a thermometer, an air-introducing tube, and a vacuum pump with a cooling trap. With stirring, 500 g of vinyloxybutyl glycidyl ether synthesized in Example 1 was gradually added to the flask while the liquid temperature was controlled to be kept at 40° C. After the addition was completed, the pressure was reduced to 20 kPa. The mixture was continuously stirred for 1 hour while dry air was introduced at 100 ml/minute. The reaction liquid was then analyzed by gas chromatography. As a result, no peak was observed for vinyloxybutyl glycidyl ether. Subsequently, 26 g of a 0.04% sodium hydrogen sulfate aqueous solution was added to the reaction liquid. While the temperature was kept at 40° C., the mixture was subjected to an acetal decomposition reaction at a pressure of 5 kPa. After 1 hour, the reaction was completed. After 2.1 g of sodium hydrogen carbonate was added to neutralize the completed reaction liquid, the liquid was concentrated by removing water from the system by distillation using a rotary evaporator. After it was checked that the content of water in the system was 800 ppm or less, the liquid concentrate was filtered and then subjected to distillation (0.4 kPa, distillation temperature 82° C.) using a reduced-pressure distillation apparatus with a Vigreux column, so that butanediol glycidyl ether was obtained with a purity of 99% and a yield of 94%. At the time, the resulting product contained 0.03% of butanediol, and no acetal dimer was detected.

Provenance & Evidence