HRID1184890

反应详情

EQUATION

反应方程式

HRID 1184890 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

Nitrogen (gas) was bubbled through the solution of methyl 3-bromobenzoate (50 mg, 0.233 mmol), potassium carbonate (96 mg, 0.698 mmol) and 3-thiopheneboronic acid (59.5 mg, 0.465 mmol) in dioxane (2 mL) and Water (0.2 mL) for 5 minutes. tetrakis(triphenylphosphine)palladium(0) (26.9 mg, 0.023 mmol) was added and again nitrogen was bubbled through the solution for 5 minutes. The reaction mixture was heated overnight at 100° C. and concentrated to dryness. Purified by chromatography (20% EtOAc in heptane) gave compound methyl 3-(thiophen-3-yl)benzoate 82 (50 mg, 99%). (m/z)=219 (M+H)+.

WORKUP

后处理

  1. customagain nitrogen was bubbled through the solution for 5 minutes
  2. concentrationconcentrated to dryness
  3. customPurified by chromatography (20% EtOAc in heptane)