HRID1243217

反应详情

EQUATION

反应方程式

HRID 1243217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Fluoro-3-methoxybenzoic acid methyl ester (2.55 g, 13.85 mmol) (from Example 34a supra) was dissolved in a mixture of tetrahydrofuran (140 mL) and water (70 mL). Lithium hydroxide monohydrate (5.8 g, 138.5 mmol) was added and the mixture was heated at reflux for 3.5 hours. After quenching with 1 N aqueous hydrochloric acid (150 mL), the solution was extracted with dichloromethane. The phases were separated and the organic layer was dried over anhydrous sodium sulfate. Concentration under reduced pressure gave 4-fluoro-3-methoxybenzoic acid as an off-white solid. (Yield 2.26 g, 96%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 3.5 hours
  3. customAfter quenching with 1 N aqueous hydrochloric acid (150 mL)
  4. extractionthe solution was extracted with dichloromethane
  5. customThe phases were separated
  6. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  7. concentrationConcentration under reduced pressure