反应详情

温度

140 °C

In a 300 ml egg plant type flask, 26 g (102 mmol) of pentaerythritol (available from Tokyo Chemical Industry, Co., Ltd.), 54 g (450 mmol) of 3-mercaptobutanoic acid (available from Yodo Chemical Co., Ltd.), 2.6 g (13.5 mmol) of p-toluenesulfonic acid monohydrate (available from Junsei Chemical Co., Ltd.) and 100 g of toluene (available from Junsei Chemical Co., Ltd.) were placed, and a Dean-Stark device and a cooling tube were installed. The contents in the flask were heated at an oil bath temperature of 140° C. with stirring. After 4 hours from the initiation of reaction, the reaction solution was allowed to cool, washed with ion-exchanged water and then neutralized with a saturated sodium hydrogencarbonate aqueous solution. The resulting solution was further washed with ion-exchanged water three times and then subjected to dehydration-drying using anhydrous magnesium sulfate (available from Junsei Chemical Co., Ltd.). Next, toluene was distilled off, and the remainder was subjected to column chromatography by a silica gel to perform purification of PEMB. As the silica gel, Wako Gel C-200 (available from Wako Pure Chemical Industries, Ltd.) was used, and as the elution solvent, n-hexane/acetone (7/1 by volume) was used. The PEMB obtained by purification was a colorless transparent liquid, and the yield was 24.5 g (21%).

1. customAfter 4 hours from the initiation of reaction
2. temperatureto cool
3. washwashed with ion-exchanged water
4. washThe resulting solution was further washed with ion-exchanged water three times
5. customto dehydration-drying
6. distillationNext, toluene was distilled off
7. custompurification of PEMB