HRID2063781

反应详情

EQUATION

反应方程式

HRID 2063781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

4-methylphenylboric acid (1.35 g, 9.91 mmol), tetrakis(triphenylphosphine)palladium (382 mg, 0.331 mmol), an aqueous solution of 2N sodium carbonate (4.5 mL) and ethanol (83 mL) were sequentially added to a solution of dimethoxyethane (9 mL) containing 6-bromo-2,2-dimethyl-2,3-dihydro-1-benzofuran (1.50 g, 6.61 mmol) synthesized in Reference Example 7, and the mixture was stirred under microwave irradiation at 150° C. for 10 minutes. After cooled to room temperature, water was added to the reaction solution, and extraction was performed using ethyl acetate. The extract was washed with saturated sodium hydrogencarbonate and saturated saline, and then dried using anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate 99:1 to 93/7) to give 880 mg of the title compound (yield: 56%).

WORKUP

后处理

  1. customsynthesized in Reference Example 7
  2. temperatureAfter cooled to room temperature
  3. washThe extract was washed with saturated sodium hydrogencarbonate and saturated saline
  4. customdried
  5. customThe solvent was removed under reduced pressure
  6. customthe obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate 99:1 to 93/7)