HRID639235

反应详情

EQUATION

反应方程式

HRID 639235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

To the 2-methoxy-2′-methyl-biphenyl-4-carboxylic acid methyl ester of step C (26 mmol) was added methanol (10 mL), tetrahydrofuran (45 mL) and 1 N sodium hydroxide (33 mL). The solution was refluxed vigorously in an oil bath at 105° C. for one hour. The volatile solvents were evaporated and the solution was chilled in ice. 2N hydrochloric acid was added until the pH was ˜1. The product was extracted into ethyl acetate, dried with anhydrous magnesium sulfate, and evaporated to a white solid. This was recrystallized from ethyl acetate/hexane to afford 5.5 g of title compound (86%).

WORKUP

后处理

  1. customThe volatile solvents were evaporated
  2. temperaturethe solution was chilled in ice
  3. addition2N hydrochloric acid was added until the pH was ˜1
  4. extractionThe product was extracted into ethyl acetate
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customevaporated to a white solid
  7. customThis was recrystallized from ethyl acetate/hexane