HRID33816

反应详情

EQUATION

反应方程式

HRID 33816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-[4-(Benzyloxy)phenyl]ethanethiol (334 mg, 1.4 mmol), methyl 2-chloro-3-[4-(2-{4-[(methylsulfonyl)oxy]phenoxy}ethyl)phenyl]propanoate (394 mg, 0.95 mmol) and potassium carbonate (189 mg, 1.4 mmol) were dissolved in 14 ml dry DMF and stirred under nitrogen atmosphere at room temperature overnight. The solvent was evaporated under reduced pressure and the residue was dissolved in toluene. The organic phase was washed (water, brine), dried (MgSO4) and evaporated. Futher purification by preparative HPLC using a gradient of CH3CN/5% CH3CN-waterphase containing 0.1M NH4OAc gave 477 mg of the desired product (yield 75%).

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in toluene
  3. washThe organic phase was washed (water, brine)
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. custompurification by preparative HPLC
  7. additioncontaining 0.1M NH4OAc