反应详情

温度

0 °C

A solution of 1.37-B of Step 2 (367 mg, 0.66 mmol) in methylene chloride (7.6 mL) was treated with triethylamine (274 μL, 2.0 mmol) followed by trichloroacetyl chloride (117 μL, 1.1 mmol) at 0° C. The reaction mixture was stirred at 0° C. for 2 h, diluted with ethyl acetate (25 mL), washed with water (2×20 mL) and brine (20 mL), dried with sodium sulfate, filtered, and concentrated to a crude residue which was purified by flash column chromatography to yield the desired product (158 mg, 45%). LCMS found for C23H26F3N4O5S2 (M+NH4)+: m/z=559.

1. washwashed with water (2×20 mL) and brine (20 mL)
2. dry with materialdried with sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated to a crude residue which
5. customwas purified by flash column chromatography