反应详情

温度

80 °C

1.07 g of 1-acetyl-3-[1-chloro-1-(4-cyanophenyl)methylene]-6-chloro-2-indolinone (starting material VII) and 0.54 g of 4-(dimethylaminomethyl)aniline (starting material IX.4) are dissolved in 10 ml of dimethylformamide and stirred at 80° C. for 3 hours. After cooling, 1 ml of 6N aqueous sodium hydroxide is added, and the mixture is stirred at room temperature for 30 minutes. Water is added and the mixture is extracted three times with methylene chloride. The combined organic phases are washed twice with water, dried over sodium sulphate and concentrated using a rotary evaporator, and the product is recrystallized from diethyl ether.

1. temperatureAfter cooling
2. stirringthe mixture is stirred at room temperature for 30 minutes
3. extractionthe mixture is extracted three times with methylene chloride
4. washThe combined organic phases are washed twice with water
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated
7. customa rotary evaporator
8. customthe product is recrystallized from diethyl ether