反应详情

0.020 ml 3-methoxy-propionic acid (0.2 mmol) and 40 mg 1′1-carbonyldiimidazole (0.24 mmol) were refluxed in 4 ml dichloromethane under nitrogen for 40 minutes. 100 mg of 5-fluoro-2-phenoxymethyl-6-piperazin-1-yl-1-(4-trifluoromethoxy-benzyl)-1H-benzoimidazole (0.2 mmol) were added and the resulting mixture refluxed for additional 4.5 h. The reaction mixture was then diluted with dichloromethane, washed with water, saturated sodium bicarbonate and brine, dried with magnesium sulfate, filtered and concentrated in vacuo, leading to 129 mg yellow solid. This residue was purified by column chromatography (40 g silicagel, dichloromethane/methanol 24:1) leading to 44 mg off-white solid (37%). MS (ISP) 587.2 (M+H)+.

1. temperaturethe resulting mixture refluxed for additional 4.5 h
2. washwashed with water, saturated sodium bicarbonate and brine
3. dry with materialdried with magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThis residue was purified by column chromatography (40 g silicagel, dichloromethane/methanol 24:1)