反应详情

温度

95 °C

To polyphosphoric acid (932 g) at 70° C. on the steam bath is added p-fluoro-α-methylhydrocinnamic acid (93.2 g, 0.5 mole) slowly with stirring. The temperature is gradually raised to 95° C., and the mixture is kept at that temperature for 1 hour. The mixture is allowed to cool and added to 2 liters of water. The aqueous layer is extracted with ether, the ether solution washed twice with saturated sodium chloride solution, 5% Na2CO3 solution, water, and then dried. The ether filtrate is concentrated with 200 g silica-gel, and added to a five pound silica-gel column packed with 5% ether-petroleum ether. The column is eluted with 5-10% ether-petroleum ether and followed by TLC to give 6-fluoro-2-methylindanone.

1. temperatureto cool
2. extractionThe aqueous layer is extracted with ether
3. washthe ether solution washed twice with saturated sodium chloride solution, 5% Na2CO3 solution, water
4. customdried
5. concentrationThe ether filtrate is concentrated with 200 g silica-gel
6. additionadded to a five pound silica-gel column
7. washThe column is eluted with 5-10% ether-petroleum ether