HRID336234

反应详情

EQUATION

反应方程式

HRID 336234 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A suspension of methyl 4-bromo-3-methylbenzoate (ABCR AV19078; 3 g; 13.10 mmol; 1 eq.), 2-(trifluoromethyl)phenylboronic acid (Aldrich 393606; 2.74 g; 14.41 mmol; 1.10 eq.), potassium carbonate (9.05 g; 65.48 mmol; 5 eq.) and tetrakis(triphenylphosphine)palladium(0) (1.51 g; 1.31 mmol; 0.10 eq.) in toluene (15 mL) and water (15 mL) was refluxed for 3 hours. The resulting mixture was filtered through a short pad of Celite, which was further washed with toluene. After evaporation of the solvent, the residue was taken up in ethyl acetate and washed successively with sat. aq. NaHCO3, water and brine, dried over magnesium sulfate and concentrated in vacuo to afford the title compound (3.7 g, 96%) as a brown oil.

WORKUP

后处理

  1. temperaturewas refluxed for 3 hours
  2. filtrationThe resulting mixture was filtered through a short pad of Celite, which
  3. washwas further washed with toluene
  4. customAfter evaporation of the solvent
  5. washwashed successively with sat. aq. NaHCO3, water and brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated in vacuo