反应详情

温度

60 °C

To a suspension of 0.012 g (0.04 mmol) of a dispersion of 60% NaH in 0.5 mL of DMF, a solution of 0.042 g (0.01 mmol)of 2-(2-{4-[1-(2-hydroxy-ethyl)-1H-indol-3-yl]-piperidin-1-yl}-ethoxy)-benzoic acid in 0.5 mL of DMF was added. After stirring at room temperature for 30 minutes as solution of 0.014 g (0.12 mmol) of allyl bromide in 0.3 mL of DMF was added. The crude mixture was stirred at room temperature for 15 hours. The solvent was evaporated at reduced pressure and the crude mixture was dissolved in 1 mL of ethanol. 0.2 mL of an aqueous 2N NaOH solution were added and the mixture was heated at 60° C. for 3 hours. The solvent was removed under reduced pressure and after addition of 1 mL of water, the mixture was neutralised with 2N HCl and extracted with chloroform. The crude was purified by chromatography over silica gel affording 0.015 g (33% of yield) of the desired product.

1. additionwas added
2. customThe solvent was evaporated at reduced pressure
3. dissolutionthe crude mixture was dissolved in 1 mL of ethanol
4. addition0.2 mL of an aqueous 2N NaOH solution were added
5. customThe solvent was removed under reduced pressure
6. additionafter addition of 1 mL of water
7. extractionextracted with chloroform
8. customThe crude was purified by chromatography over silica gel affording 0.015 g (33% of yield) of the desired product