反应详情

温度

0 °C

To a stirred solution of 4-Methyl-5-[4-(2,2,2-trifluoro-acetyl)-piperazin-1-yl]-benzofuran-2-carboxylic acid ethyl ester (0.15 g, 0.0003 mol) in dry THF was added triethyl amine (0.15 ml, 0.001 mol) and cooled to 0° C. and stirred under nitrogen. 2,6 dichloro benzyl bromide (0.107 g, 0.00045 mol) was added and stirred for 2 hours at room temperature. The completion of the reaction was confirmed by TLC. Solvent was concentrated under reduced pressure added water. The solid separated was filtered, washed with water (10 ml). After drying under vacuum, the crude product was isolated as brown solid. Column chromatography using 10/90 ethyl acetate/hexane yielded 5-[4-(2,6-Dichloro benzyl)-piperazine-1-yl]-4-methyl-benzofuran-2-carboxylic acid ethyl ester (0.13 g, 78%).

1. stirringstirred for 2 hours at room temperature
2. concentrationSolvent was concentrated under reduced pressure
3. additionadded water
4. customThe solid separated
5. filtrationwas filtered
6. washwashed with water (10 ml)
7. customAfter drying under vacuum
8. customthe crude product was isolated as brown solid