HRID1949331

反应详情

EQUATION

反应方程式

HRID 1949331 的结构方程式

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

4.5 g of anhydrous aluminium chloride (33.7 mmol) are introduced, under a nitrogen atmosphere, at ambient temperature and with stirring, into 10.37 g of tributylamine (56 mmol) in a three-necked round-bottomed flask. The medium is brought to 60° C. and is maintained at this value for 4 h. 1 g of (E)-3,5,4′-trimethoxystilbene (3.7 mmol) is then introduced and the reaction medium is brought to 80° C. for 2 h and to 100° C. for 2 h. It is brought back to ambient temperature and then 10 g of a 50/50 water/ice mixture are added. It is maintained at 0-5° C. with stirring for 3 h and extracted 4 to 5 times with 10 ml of methyl ethyl ketone. The combined organic phases are washed with 10 ml of a saturated aqueous sodium bicarbonate solution and then with 10 ml of water. After concentrating the organic phase, an HPLC quantitative determination (external calibration) gives an (E)-resveratrol yield of 75%.

WORKUP

后处理

  1. customis brought to 60° C.
  2. temperatureis maintained at this value for 4 h
  3. customis brought back to ambient temperature
  4. extractionextracted 4 to 5 times with 10 ml of methyl ethyl ketone
  5. washThe combined organic phases are washed with 10 ml of a saturated aqueous sodium bicarbonate solution
  6. concentrationAfter concentrating the organic phase