反应详情

To a solution of 48 mg (0.3 mmol) of 1H-indole-7-carboxylic acid and 96 mg of TBTU (0.3 mmol) in 4 ml DMF, were added 0.26 ml (1.5 mmol) of N,N-diisopropylethyl amine. After stirring for 5 min at rt, 95 mg (0.3 mmol) (4-tert-butyl-benzyl)-[2-(3,4-dichloro-phenyl)-ethyl]-amine in 1 ml DMF was added. After 1.5 h stirring 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 yellow solid foam was purified by column chromatography (8 g silica gel; heptane/EtOAc 9:1) to give 137 mg (94%) of a white solid. MS (ISP) 479.5 (M+H)+.

1. stirringAfter 1.5 h stirring 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 yellow solid foam was purified by column chromatography (8 g silica gel; heptane/EtOAc 9:1)