反应详情

温度

24 °C

To a DMF solution (10 mL) of (S)-4-dibenzofuran-2-yl-4-oxo-2-(2,2,2-trifluoroacetylamino)-butyric acid (0.3 g, 0.00079 mol) at 40° C. was added carbonyldimidazole (0.13 g, 0.00079 mol). This mixture was stirred for 1 hour and then 1,8-diazabicyclo-[5.4.0]undec-7-ene (DBU, 0.12 mL, 0.00079 mol) and t-butanol (0.15 mL, 0.00158 mol) were added. The reaction mixture was stirred for 24 hours at 40° C., cooled to 24° C., and then diluted with ether (20 mL). The solution was washed with water (2×10 mL), brine (2×10 mL), and dried over anhydrous magnesium sulfate. The mixture was filtered and the filtrate was concentrated to an oil by evaporation of the solvent in vacuo. The oil was flash chromatographed on silica gel eluting with 20% ethyl acetate/hexane (v/v) to yield the title compound; mp 92-94° C.

1. stirringThe reaction mixture was stirred for 24 hours at 40° C.
2. washThe solution was washed with water (2×10 mL), brine (2×10 mL)
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationThe mixture was filtered
5. concentrationthe filtrate was concentrated to an oil by evaporation of the solvent in vacuo
6. customchromatographed on silica gel eluting with 20% ethyl acetate/hexane (v/v)