反应详情

To a suspension of sodium hydride (80 mg, 1.96 mmole, 60%) in dimethyl sulfoxide (1 ml) was added a solution of intermediate 2 obtained in Referential Example 2 (350 mg, 0.98 mmole) at room temperature under nitrogen, and the reaction mixture was stirred for 10 minutes. The resulting mixture was added dropwise to a solution of α,α'-dichloro-m-xylene (172 mg, 0.98 mmole) in dimethyl sulfoxide (1 ml) at room temperature, and stirred for 2 hours. The reaction mixture was chilled in ice, diluted with water, and extracted with ethyl acetate. The combined organic layers were dried over MgSO4, and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel/ethyl acetate) to give the desired compound (387 mg) as a pale yellow oil.

1. stirringstirred for 2 hours
2. temperatureThe reaction mixture was chilled in ice
3. extractionextracted with ethyl acetate
4. dry with materialThe combined organic layers were dried over MgSO4
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography (silica gel/ethyl acetate)