HRID377310

反应详情

EQUATION

反应方程式

HRID 377310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium carbonate (11.13 g) was added portionwise to a stirred solution of dihydroxy-(3-methoxyphenyl)borane (5.85 g) and 3-iodobenzoic acid (8.68 g) in water (138 ml) at room temperature, and then palladium(II) acetate (78.6 mg) was added portionwise thereto at the same temperature. The resulting mixture was stirred at the same temperature for 4 hours. The reaction mixture was filtered, then the filtrate was washed twice with diethyl ether and adjusted to pH 2.0 with 6N hydrochloric acid. The precipitated powder was collected by filtration and dissolved in ethyl acetate. The solution was dried over magnesium sulfate and evaporated in vacuo. The residue was washed with n-hexane to afford 3'-methoxy-3-biphenylcarboxylic acid (4.34 g) as a powder.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. washthe filtrate was washed twice with diethyl ether
  3. filtrationThe precipitated powder was collected by filtration
  4. dissolutiondissolved in ethyl acetate
  5. dry with materialThe solution was dried over magnesium sulfate
  6. customevaporated in vacuo
  7. washThe residue was washed with n-hexane