反应详情

温度

0 °C

A stirred mixture of 2,3-dimethylanisole (6.8 g., 0.05 mole) and 2,2-diethylmalonyl chloride (10 g., 0.051 mole) in hexane (75ml.) is cooled to 0°C. and treated with aluminum chloride (13.5 g., 0.11 mole) in several portions over a 15 minute period. The reaction is heated at reflux for 2 hours, the hexane is distilled at reduced pressure, the product treated with cold 1N-hydrochloric acid, extracted into ether, washed with water, 5% sodium hydroxide, water then dried over magnesium sulfate. Evaporation of the ether at reduced pressure affords 6.3 g. of 2,2-diethyl-4,5-dimethyl-6-methoxy-indan-1,3-dione which melts at 80°-81°C. after recrystallization from petroleum ether.

1. temperatureThe reaction is heated
2. temperatureat reflux for 2 hours
3. distillationthe hexane is distilled at reduced pressure
4. additionthe product treated with cold 1N-hydrochloric acid
5. extractionextracted into ether
6. washwashed with water, 5% sodium hydroxide, water
7. dry with materialthen dried over magnesium sulfate
8. customEvaporation of the ether at reduced pressure
9. customaffords 6.3 g
10. customof 2,2-diethyl-4,5-dimethyl-6-methoxy-indan-1,3-dione which melts at 80°-81°C. after recrystallization from petroleum ether