HRID639235
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe volatile solvents were evaporated
- temperaturethe solution was chilled in ice
- addition2N hydrochloric acid was added until the pH was ˜1
- extractionThe product was extracted into ethyl acetate
- dry with materialdried with anhydrous magnesium sulfate
- customevaporated to a white solid
- customThis was recrystallized from ethyl acetate/hexane