HRID1942600

反应详情

EQUATION

反应方程式

HRID 1942600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of (2-methylpropyl)boronic acid (0.508 g), methyl 3-cyano-4-{[(trifluoromethyl)sulfonyl]oxy}benzoate (D22) (1.4 g) and Cs2CO3 (4.43 g) in toluene (10 mL) and water (1 mL) stirred under nitrogen at room temperature was added PdCl2(dppf)-CH2Cl2 adduct (0.370 g). The reaction mixture was stirred at 100° C. for 12 h. The solvent was removed under reduced pressure. The residue was dissolved in EA (80 mL) and washed with water and brine, dried over anhydrous Na2SO4. The solution was concentrated and the crude product was purified by column chromatography to afford methyl 3-cyano-4-(2-methylpropyl)benzoate (D23) (800 mg) as a colorless oil. MS (ES): C13H15NO2 requires 217. found 218.1 (M+H+).

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in EA (80 mL)
  3. washwashed with water and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationThe solution was concentrated
  6. customthe crude product was purified by column chromatography