反应详情

温度

150 °C

To a dimethylsulfoxide (10 ml) solution of potassium t-butoxide (262 mg, 2.33 mmol) and 2-mercaptobenzimidazole (349 mg, 2.33 mmol), (4-((2,2-dimethyl-1,3-dioxan-5-yl)methoxy)-3,5-dimethylpyridin-2-yl)methyl acetate (500 mg, 1.55 mmol) was added and the mixture was stirred in a nitrogen atmosphere at 150° C. for 3 hours and 10 minutes. After cooled to room temperature, the reaction mixture was diluted with toluene and washed with a diluted aqueous sodium hydroxide solution and a saturated saline solution, dried over sodium sulfate, and filtrated. The filtrate was concentrated under reduced pressure. The residue was subjected twice to silica gel column chromatography (elution solvent: n-heptane/ethyl acetate=1/1) to obtain the title compound (441 mg, 68.8%) as a white foam.

1. temperatureAfter cooled to room temperature
2. washwashed with a diluted aqueous sodium hydroxide solution
3. dry with materiala saturated saline solution, dried over sodium sulfate
4. filtrationfiltrated
5. concentrationThe filtrate was concentrated under reduced pressure
6. washThe residue was subjected twice to silica gel column chromatography (elution solvent: n-heptane/ethyl acetate=1/1)