HRID558129
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
Add thionyl chloride (1.5 g, 12.6 mmol) to a solution of (2-bromo-4-fluoro-phenyl)-acetic acid (0.3 g, 1.26 mmol) in DCM (3 mL). Reflux the mixture for 2 h. Remove the solvent and excess thionyl chloride under reduced pressure to give the intermediate (2-bromo-4-fluorophenyl)-acetyl chloride. Dissolve the residue in DCM (3 mL) and add to a stirred solution of ethanolamine (0.15 mL, 2.52 mmol) in DCM (3 mL) at 0° C. Stir the mixture overnight. Dilute with DCM and wash with saturated NaHCO3, water, and aqueous saturated sodium chloride. Dry over sodium sulfate. Concentrate the solution in vacuo to give the title compound as a white solid (300 mg, 86%). MS (ES) m/z 276 [M+1]+.
WORKUP
后处理
- temperatureReflux the mixture for 2 h
- customRemove the solvent and excess thionyl chloride under reduced pressure