反应详情

温度

100 °C

To a stirred solution of 2.97 g of 3,6-dimethylcatechol and 3.86 g of potassium carbonate in 60 mL of N,N-dimethylformamide is added 1.69 mL of bromochloromethane. A reflux condenser is attached and the mixture heated in an oil bath to 100° C. for 24 hours. The mixture is allowed to cool to room temperature and then is distributed between 100 mL of water and 200 mL of ether. The aqueous layer is separated and extracted with ether. The combined ether layers are dried over magnesium sulfate and concentrated under reduced pressure to yield a red liquid, which is purified by chromatography on silica gel to afford 2.0 g of 4,7-dimethyl-1,3-benzodioxole as a light yellow liquid.

1. customA reflux condenser is attached
2. temperatureto cool to room temperature
3. customThe aqueous layer is separated
4. extractionextracted with ether
5. dry with materialThe combined ether layers are dried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customto yield a red liquid, which
8. customis purified by chromatography on silica gel