反应详情

温度

0 °C

To a solution of 260 mg (0.543 mmol) of 2-((3R,5R,6S)-5-(3-chlorophenyl)-6-(4-chlorophenyl)-1-((2S,3S)-2-hydroxypentan-3-yl)-3-methyl-2-oxopiperidin-3-yl)acetic acid (Example 152) in 5 mL of THF was added 60% sodium hydride (217 mg, 5.43 mmol) at 0° C. After being stirred at 0° C. for 20 min, iodomethane (271 uL, 4.35 mmol) was added. The reaction was allowed to warm to ambient temperature, and stirred for an additional 3 h until completion. The reaction was quenched with saturated aqueous NH4Cl solution, extracted with EtOAc (2×25 mL). The combined organic layers were washed with saturated NaCl, dried over MgSO4, filtered and the filtrate was concentrated to provide the title compound.

1. temperatureto warm to ambient temperature
2. stirringstirred for an additional 3 h until completion
3. customThe reaction was quenched with saturated aqueous NH4Cl solution
4. extractionextracted with EtOAc (2×25 mL)
5. washThe combined organic layers were washed with saturated NaCl
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationthe filtrate was concentrated