反应详情

温度

20 °C

Triethylsilane (5 ml) was added to a stirred solution of 2-[4-[4-(2-methyl-tetrazol-5-yl)-2,6-dimethylphenoxy]-1-hydroxy-butyl]-7-azaindole (520 mg, 1.33 mmol) in 20 ml of trifluoroacetic acid at 20° C. under nitrogen. The mixture was stirred at 20° C. for 10 min and then stirred at 70°-75° C. for 16 h. To the mixture was added water, and basified with an aqueous sodium bicarbonate solution (to pH=8) followed by extraction with methylene chloride (3×). The combined organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica column chromatography (7.5 cm column, ethyl acetate/hexane, 1/5-8/1). The mixture was recrystallized to afford 349 mg (74%) of 2-[4-[4-(2-methyl-tetrazol-5-yl)-2,6-dimethylphenoxy]-butyl]-7-azaindole, as a white solid, m.p.147°-150° C.

1. stirringstirred at 70°-75° C. for 16 h
2. extractionfollowed by extraction with methylene chloride (3×)
3. dry with materialThe combined organic layer was dried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was purified by silica column chromatography (7.5 cm column, ethyl acetate/hexane, 1/5-8/1)
6. customThe mixture was recrystallized