HRID643204

反应详情

EQUATION

反应方程式

HRID 643204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Decanoic acid (2.00 g, 11.61 mmol), vanillyl alcohol (1.74 g, 11.27 mmol), and Novozym 435 (100 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 20 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 reaction mixture was returned to room temperature, hexane (50 ml) was added, and Novozym 435 and a small amount of precipitated vanillyl alcohol were removed by filtration. The filtrate was washed with 5% aqueous citric acid solution (25 ml) and saturated brine (25 ml), and dried over anhydrous magnesium sulfate. Magnesium sulfate was removed by filtration, and the filtrate was concentrated under reduced pressure to give a mixture (3.41 g) of vanillyl decanoate and decanoic acid as a colorless oil. As a result of the analysis, the yield of vanillyl decanoate was 94.1%. The mixture contained 6.0 wt % of decanoic acid relative to vanillyl decanoate.

WORKUP

后处理

  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. customNovozym 435 and a small amount of precipitated vanillyl alcohol were removed by filtration
  7. washThe filtrate was washed with 5% aqueous citric acid solution (25 ml) and saturated brine (25 ml)
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customMagnesium sulfate was removed by filtration
  10. concentrationthe filtrate was concentrated under reduced pressure