反应详情

温度

25 °C

To a solution of (3S,5R,6S)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)-3-methyl-1-((S)-1-(methylamino)butan-2-yl)piperidin-2-one (72 mg, 0.16 mmol; Example 134 Step A) in DMF (0.40 mL) was added methanesulfonyl chloride (61 μL, 0.79 mmol) and pyridine (76 μL, 0.95 mmol) successively at 0° C. After being stirred at 25° C. for overnight, the reaction was acidified (10% citric acid) and extracted (2×EtOAc). The combined organic layers were washed (sat. aq. NaCl solution), dried (Na2SO4), and concentrated under reduced pressure. Separation by RP-HPLC (50 to 85% MeCN/H2O (0.1% TFA) a gradient elution) provided the title compound as a pale yellow film.

1. extractionextracted (2×EtOAc)
2. washThe combined organic layers were washed (sat. aq. NaCl solution)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated under reduced pressure
5. customSeparation by RP-HPLC (50 to 85% MeCN/H2O (0.1% TFA)
6. washa gradient elution)