反应详情

温度

0 °C

A solution containing 35 (228 mg, 0.4 mmol), DIPEA (104 mg, 0.8 mmol) and DMAP (cat) in DCM (5 mL) was cooled to 0° C. Methanesulfonyl chloride (55 mg, 0.48 mmol) was added. After 1 h, the reaction mixture was warmed to ambient temperature, diluted with DCM, washed successively with saturated aqueous NaHCO3, 1N HCl, and brine, dried over anhydrous Na2SO4, filtered, and concentrated. The crude product was purified by RP-HPLC (2″ Dynamax® C18; 10-100% ACN/water containing 0.1% HOAc over 30 min; Flow: 40 mL/min) to afford compound 36 (190 mg) as a white solid. Mass spectrum, m/z [651.1] (M+H)+.

1. temperaturethe reaction mixture was warmed to ambient temperature
2. washwashed successively with saturated aqueous NaHCO3, 1N HCl, and brine
3. dry with materialdried over anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product was purified by RP-HPLC (2″ Dynamax® C18
7. wait10-100% ACN/water containing 0.1% HOAc over 30 min