HRID2104608

反应详情

EQUATION

反应方程式

HRID 2104608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-[3-phenyl-8-(trifluoromethyl)quinolin-4-yl]phenol (0.178 g, 0.487 mmol), and potassium carbonate (0.134 g, 0.974 mmol), in DMF at 120° C. is added 4-bromomethylphenylacetic acid ethyl ester (0.334 g, 1.46 mmol), drop wise over 2 h. After an additional 2 h, the cooled reaction is poured into 2N aq HCl and extracted with ethyl acetate. The combined extracts are washed with sat aq NaHCO3, water, brine, and dried with magnesium sulfate. The extracts are concentrated and the residue is chromatographed with 1:9 ethyl acetate:hexanes to afford the title compound as a syrup (0.051 g, 37%). MS m/z 542; HRMS: calcd for C33H26NF3O3+H, 542.19430; found (ESI, [M+H]+), 542.194.

WORKUP

后处理

  1. waitAfter an additional 2 h
  2. customthe cooled reaction
  3. extractionextracted with ethyl acetate
  4. washThe combined extracts are washed with sat aq NaHCO3, water, brine
  5. dry with materialdried with magnesium sulfate
  6. concentrationThe extracts are concentrated
  7. customthe residue is chromatographed with 1:9 ethyl acetate