HRID406981

反应详情

EQUATION

反应方程式

HRID 406981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

4,4,5,5-Tetramethyl-1,3,2-dioxaborolane (1.3 mL, 9.0 mmol) was added to a mixture of ethyl 2-(4-bromophenyl)propanoate (1.3 g, 5.0 mmol), bis(acetonitrile)palladium(II) chloride (26 mg, 0.10 mmol), 2-(dicyclohexylphosphino)-2′,6′-dimethoxy-1,1′-biphenyl (160 mg, 0.40 mmol) and triethylamine (2.1 mL, 15 mmol) in 1,4-dioxane (3.0 mL) and then the mixture was evacuated under reduced pressure and then refilled with nitrogen thrice. The reaction was then heated at 110° C. for 4 h. The mixture was cooled to r.t. and filtered through a short pad of silical gel and then washed with ethyl acetate. The solvent was removed under reduced pressure. The residue was purified by flash chromatography on a silica gel column eluting with ethyl acetate in hexane (0-10%) to afford the desired product.

WORKUP

后处理

  1. customthe mixture was evacuated under reduced pressure
  2. additionrefilled with nitrogen thrice
  3. temperatureThe mixture was cooled to r.t.
  4. filtrationfiltered through a short pad of silical gel
  5. washwashed with ethyl acetate
  6. customThe solvent was removed under reduced pressure
  7. customThe residue was purified by flash chromatography on a silica gel column
  8. washeluting with ethyl acetate in hexane (0-10%)