反应详情

0.020 ml of cyclopropyl-acetic acid (0.2 mmol) and 40 mg of 1,1-carbonyldiimidazole (0.24 mmol) were refluxed in 4 ml dichloromethane under nitrogen for 40 minutes. 100 mg 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 26 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 (24 g silicagel, dichloromethane/methanol 24:1) leading to 77 mg light yellow solid (63%). MS (ISP) 583.3 (M+H)+.

1. temperaturethe resulting mixture refluxed for additional 26 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 (24 g silicagel, dichloromethane/methanol 24:1)