HRID33816
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent was evaporated under reduced pressure
- dissolutionthe residue was dissolved in toluene
- washThe organic phase was washed (water, brine)
- dry with materialdried (MgSO4)
- customevaporated
- custompurification by preparative HPLC
- additioncontaining 0.1M NH4OAc