反应详情

温度

50 °C

Decanoic acid (25.0 g, 145 mmol), vanillyl alcohol (21.7 g, 141 mmol), and Novozym 435 (723 mg) were measured and placed in a flask (25 ml). The mixture in the flask free of a plug was heated with stirring in an oil bath at 50° C. for 48 hours. After 2 to 3 hours of stirring with heating, attachment of water on the wall of the upper part of the flask was observed. The flask was returned to room temperature, hexane (100 ml) was added to the reaction mixture, and the mixture was stirred for 1 hour. The immobilized enzyme and a small amount of precipitated vanillyl alcohol were removed by filtration. Hexane (100 ml) and 10% aqueous citric acid solution (200 ml) was added to the filtrate to allow partitioning. The aqueous layer was further extracted with hexane (150 ml), and the combined hexane layer was washed with 10% aqueous citric acid solution (100 ml), water (100 ml) and saturated brine (100 ml). The hexane layer was dried over anhydrous magnesium sulfate. Magnesium sulfate was removed by filtration, and the filtrate was concentrated under reduced pressure to give the mixture (43.7 g) of vanillyl decanoate and decanoic acid. As a result of the analysis, the yield of vanillyl decanoate was 97.0% and the purity was 98.6 area % by HPLC. The mixture contained 3.94 wt % of decanoic acid relative to vanillyl decanoate.

1. customplaced in a flask
2. temperatureThe mixture in the flask free of a plug was heated
3. stirringAfter 2 to 3 hours of stirring
4. temperaturewith heating
5. customwas returned to room temperature
6. stirringthe mixture was stirred for 1 hour
7. customThe immobilized enzyme and a small amount of precipitated vanillyl alcohol were removed by filtration
8. additionHexane (100 ml) and 10% aqueous citric acid solution (200 ml) was added to the filtrate
9. customto allow partitioning
10. extractionThe aqueous layer was further extracted with hexane (150 ml)
11. washthe combined hexane layer was washed with 10% aqueous citric acid solution (100 ml), water (100 ml) and saturated brine (100 ml)
12. dry with materialThe hexane layer was dried over anhydrous magnesium sulfate
13. customMagnesium sulfate was removed by filtration
14. concentrationthe filtrate was concentrated under reduced pressure