反应详情

温度

80 °C

To a suspension of 369 mg of 6-fluoro-3-[(E)-2-(3-fluorophenyl)-vinyl]-1-trityl-1H-indazole-5-carboxylic acid obtained by Production example 108 in 6 mL of toluene were added 69 mg of triethylamine, 0.15 mL of 2-methyl-2-propanol and 187 mg of diphenyl phosphoryl azide, and stirred at 80° C. for 7.5 hours. After adding 10 mL of ethyl acetate to the reaction solution, the organic layer was washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product purified and separated by silica gel column chromatography (n-hexane:toluene=1:1), to afford 102 mg of the title compound as a white non-crystalline powder.

1. washthe organic layer was washed successively with water and saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. customThe solvent was evaporated
4. customthe crude product purified
5. customseparated by silica gel column chromatography (n-hexane:toluene=1:1)