反应详情

温度

75 °C

A room temperature suspension of zinc powder (430 mg, 6.56 mmol) and dichlorodimethylsilane (0.80 mL, 6.59 mmol) in 1,2-dichloroethane (15 mL) was treated with a solution of 3,4,5-trimethoxybenzenesulfonyl chloride (500 mg, 1.87 mmol) and 1,3-dimethyl-2-imidazolidinone (647 mg, 5.67 mmol) in 1,2-dichloroethane (15 mL). The reaction was heated to 75° C. for 1 hour, cooled to room temperature, filtered, and concentrated. The concentrate was dissolved in methanol, concentrated, dissolved in methanol, and concentrated. The concentrate was purified by flash column chromatography on silica gel with dichloromethane to provide the desired product.

1. temperaturecooled to room temperature
2. filtrationfiltered
3. concentrationconcentrated
4. dissolutionThe concentrate was dissolved in methanol
5. concentrationconcentrated
6. dissolutiondissolved in methanol
7. concentrationconcentrated
8. customThe concentrate was purified by flash column chromatography on silica gel with dichloromethane