HRID2244906

反应详情

EQUATION

反应方程式

HRID 2244906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-[2-bromo-5-(trifluoromethyl)phenyl]propanoic acid (2.8 g, 9.4 mmol) in THF (100 mL) and hexane (20 mL) at −78° C. was dropwise added a 2.5 M solution of n-butyllithium in hexane (8.3 mL). After the addition had been completed, the reaction was quenched with saturated NH4Cl. The resulting solution was extracted with ethyl acetate twice. The extracts were washed with saturated NaHCO3, brine, dried over MgSO4 and concentrated. The crude material was purified by flash chromatography on silica eluting with 10-20% EtOAc/hexane to afford the desired product as a white solid (0.7 g, 37%). LC/MS calculated for C10H7F3O: (M+H)+ 201; found 201.1.

WORKUP

后处理

  1. additionAfter the addition
  2. customthe reaction was quenched with saturated NH4Cl
  3. extractionThe resulting solution was extracted with ethyl acetate twice
  4. washThe extracts were washed with saturated NaHCO3, brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. customThe crude material was purified by flash chromatography on silica eluting with 10-20% EtOAc/hexane