反应详情

To a solution of 80 mg (0.45 mmol) of 6-fluoro-1H-indole-7-carboxylic acid and 143 mg of TBTU (0.45 mmol) in 5 ml DMF, were added 0.38 ml (2.23 mmol) of N,N-diisopropylethyl amine. After stirring for 5 min at rt, 176 mg (0.58 mmol) of (4-tert-butyl-benzyl)-[2-(3,5-difluoro-phenyl)-ethyl]-amine were added. After stirring for 17 h at rt, the reaction mixture was diluted with 50 ml water and extracted with 2×50 ml EtOAc. The combined organic phases were washed with water and brine, dried with magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography (40 g silica gel; EtOAc/heptane 1:4) to give 166 mg light brown foam (78%). MS 464.1 (M)

1. stirringAfter stirring for 17 h at rt
2. extractionextracted with 2×50 ml EtOAc
3. washThe combined organic phases were washed with water and brine
4. dry with materialdried with magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by column chromatography (40 g silica gel; EtOAc/heptane 1:4)