反应详情

To a 16 ml vial was added 4-(cyclopropyloxy)-2,6-bis(methylthio)benzoic acid (375 mg, 1.39 mmol), 4-(1-methyl-1-{[3-(trifluoromethyl)phenyl]sulfonyl}ethyl)piperdine (465 mg, 1.39 mmol), Bop reagent (675 mg, 1.53 mmol), diisopropylethyl amine (1.21 ml, 6.93 mmol) and 4 ml dimethylformamide. The resulting solution was stirred at room temperature for 1 hour. It was diluted with 30 ml ethyl acetate, washed sequencially with 20 ml 1N HCl, 20 ml 5% KOH and 20 ml brine. The organics were dried over sodium sulfate, filtered and concentrated. The residue was purified on silica gel column eluted with 1:2 to 1:1 ethyl acetate/hexane to give desired product as sticky material.

1. washwashed sequencially with 20 ml 1N HCl, 20 ml 5% KOH and 20 ml brine
2. dry with materialThe organics were dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified on silica gel column
6. washeluted with 1:2 to 1:1 ethyl acetate/hexane