反应详情

温度

95 °C

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

1. temperatureto cool
2. additionis added to 2 l
3. extractionThe aqueous suspension is extracted with ether
4. washThe extract is washed twice with saturated sodium chloride solution, 5% Na2CO3 solution, and water
5. customis dried
6. concentrationis concentrated on 200 g silica-gel
7. additionthe slurry is added to a five pound silica-gel column
8. washThe column is eluted with 5-10% ether-petroleum ether