Tributylamine → Resveratrol

温度

2.5 °C

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%.

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

ORDレコード

ord-e383b14e825a47729212ae0eb6abd845

出典データセット

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08399714B2