HRID257847

反应详情

EQUATION

反应方程式

HRID 257847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the above ester (Step G), sodium hydride (3 equivalents), and dry DMF is stirred under N2 at room temperature for 2 hours. Next, benzyl bromide (5 equivalents) is added, and stirring at room temperature is continued for an additional 1.5 hours or until TLC indicates complete reaction. The mixture is quenched by cautious addition of sufficient acetic acid to destroy the excess sodium hydride and then partitioned between ethyl acetate and H2O. The ethyl acetate phase is washed repeatedly with H2O, then dried (Na2SO4), filtered, and concentrated in vacuo. Chromatography of the residue on silica gel affords the title compound.

WORKUP

后处理

  1. stirringstirring at room temperature
  2. waitis continued for an additional 1.5 hours or until TLC
  3. customreaction
  4. customThe mixture is quenched by cautious addition of sufficient acetic acid
  5. customto destroy the excess sodium hydride
  6. custompartitioned between ethyl acetate and H2O
  7. washThe ethyl acetate phase is washed repeatedly with H2O
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo