反应详情

温度

0 °C

A solution containing 50 (200 mg, 0.41 mmol) and DIPEA (163 mg, 1.26 mmol) in anhydrous DCM (5 mL) was cooled to 0° C. A solution of MsCl (44 mg, 0.41 mmol) in DCM (0.5 mL) was added followed by the addition of DMAP (5 mg, cat.). After 2 h, the reaction mixture was diluted with DCM and washed successively with 1M HCl and brine, dried over anhydrous Na2SO4, filtered, and concentrated. The crude product was purified by flash silica gel chromatography (1:1 hexanes/EtOAc) to afford 114 mg (49%) of 61 as a white solid. Mass spectrum, m/z [563] (M+H)+.

1. washwashed successively with 1M HCl and brine
2. dry with materialdried over anhydrous Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe crude product was purified by flash silica gel chromatography (1:1 hexanes/EtOAc)