反应详情

Under ice-cooling, 4.16 g of 2,5-dimethoxycinnamic acid is dissolved in 50 ml of acetonitrile, and to the resultant solution are added 3.03 g of triethylamine, then 4.13 g of diethylphosphorochloridate. After the mixture is stirred for one hour, 2.74 g of 4-amino-2,6-dimethylphenol is added and the reaction mixture is stirred at room temperature. After completion of the reaction, ice chips are added, and then 5 % aqueous sodium hydrogen carbonate solution is added. The crystals precipitated are collected by filtration, and washed with isopropyl ether. The crystals obtained are recrystallized form ethyl acetate to give 4.64 g of 4-(2,5-dimethoxycinnamoylamino)-2,6-dimethylphenol as white crystals.

1. temperatureUnder ice-cooling
2. stirringthe reaction mixture is stirred at room temperature
3. customAfter completion of the reaction, ice chips
4. additionare added
5. customThe crystals precipitated
6. filtrationare collected by filtration
7. washwashed with isopropyl ether
8. customThe crystals obtained
9. customare recrystallized form ethyl acetate