反应详情

温度

95 °C

To 932 g. polyphosphoric acid at 70° on the steam bath is added ρ-fluoro-a-methylhydrocinnamic acid (93.2 g., 0.5 mole) slowly with stirring. The temperature is gradually raised to 95° C., and the mixture kept at this temperature for 1 hour. The mixture is allowed to cool and added to 2 l. 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. additionadded to 2 l
3. extractionThe aqueous layer is extracted with ether
4. washthe ether solution washed twice with saturated sodium chloride solution, 5% Na2CO3 solution, water
5. customdried
6. concentrationThe ether filtrate is concentrated with 200 g
7. additionsilica-gel, and added to a five pound silica-gel column
8. washThe column is eluted with 5-10% ether-petroleum ether