HRID2289325
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
To a solution of 2-(2,2,2-trifluoroethoxy)-3-chlorobenzyl bromide (1.6 g, 5.4 mmol) from Step 2 above in DMF (12 mL) was added NaCN (0.28 g, 5.7 mmol). The solution was stirred at ambient temperature for 14 h. The solvent was removed under reduced pressure and the residue was partitioned between EtOAc and saturated aqueous NaHCO3. The organic phase was dried (MgSO4), filtered, and the solvent was removed under reduced pressure. The residue was purified by pressurized silica gel column chromatography using a gradient elution of 5-20% EtOAc:hexanes to give 2-(2,2,2-trifluoroethoxy)-3-chlorophenylacetonitrile as a colorless oil.
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- customthe residue was partitioned between EtOAc and saturated aqueous NaHCO3
- dry with materialThe organic phase was dried (MgSO4)
- filtrationfiltered
- customthe solvent was removed under reduced pressure
- customThe residue was purified by pressurized silica gel column chromatography
- washa gradient elution of 5-20% EtOAc