反应详情

To a solution of 43 mg (0.22 mmol) of 5,6-difluoro-1H-indole-7-carboxylic acid and 68 mg of TBTU (0.22 mmol) in 2 ml DMF, were added 0.19 ml (1.09 mmol) of N,N-diisopropylethyl amine. After stirring for 5 min at rt, 66 mg (0.22 mmol) of [rac]-(4-tert-butyl-benzyl)-[2-(4-fluoro-phenyl)-2-hydroxy-ethyl]-amine were added. After stirring for 17 h at rt, the reaction mixture was diluted with 20 ml water and extracted with EtOAc (2×). 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 (8 g silica gel; EtOAc/heptane 1:2) to give 56 mg light yellow foam (47%). MS(ISP): 481.4 (M+H)+.

1. stirringAfter stirring for 17 h at rt
2. extractionextracted with EtOAc (2×)
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 (8 g silica gel; EtOAc/heptane 1:2)