反应详情

温度

-10 °C

In 50 ml of methylene chloride is suspended 2.20 g of 5-(4'-hydroxy 3'-methoxyphenyl)pentadienoic acid under an argon atmosphere. To the suspension cooled to -10° C. are added 2.92 ml of triethylamine and 2.16 g of ethyl chlorocarbonate. To the mixture, after stirred for one hour, is added a solution of 1.28 g of prenylamine in 10 ml of methylene chloride, and the resulting mixture is stirred at -10° C. to 0° C. for 3 hours. The reaction mixture is poured onto water and extracted with chloroform. The organic layer is washed with saturated aqueous sodium chloride and dried over anhydrous sodium sulfate. The solvent is then distilled off under reduced pressure, and the residue is subjected to column chromatography on silica gel. From the fraction eluted with methylene chloride-methanol (99:1) is obtained 2.91 g of 5-(4'-ethoxycarbonyloxy-3'-methoxyphenyl)pentadienoic acid prenylamide.

1. stirringthe resulting mixture is stirred at -10° C. to 0° C. for 3 hours
2. additionThe reaction mixture is poured onto water
3. extractionextracted with chloroform
4. washThe organic layer is washed with saturated aqueous sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent is then distilled off under reduced pressure
7. washFrom the fraction eluted with methylene chloride-methanol (99:1)