HRID1048459

反应详情

EQUATION

反应方程式

HRID 1048459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 0° C. solution of (5R,6S)-1-((S)-1-(tert-butyldiphenylsilyloxy)butan-2-yl)-5-(3-chlorophenyl)-6-(4-chlorophenyl)-3-hydroxypiperidin-2-one (476 mg, 0.736 mmol; Example 203, Step A) in THF (7.360 mL) was added sodium hydride (58.9 mg, 1.472 mmol). After 30 minutes, iodomethane (0.092 mL, 1.472 mmol) was added. After 5 minutes, the cooling bath was removed. After 2 hours, the mixture was quenched with sat. aq. NH4Cl solution. The mixture was partitioned between ethyl acetate and water. The organic layer was washed with sat. aq. NaCl solution, dried over Na2SO4, and concentrated to afford the title compound.

WORKUP

后处理

  1. waitAfter 5 minutes
  2. customthe cooling bath was removed
  3. waitAfter 2 hours
  4. customthe mixture was quenched with sat. aq. NH4Cl solution
  5. customThe mixture was partitioned between ethyl acetate and water
  6. washThe organic layer was washed with sat. aq. NaCl solution
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated