HRID1773546

反应详情

EQUATION

反应方程式

HRID 1773546 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of sodium hydroxide (1.6 g, 40 mmol) in water (30 mL) was added to a solution of 7-bromo-3-methoxy-naphthalene-2-carboxylic acid methyl ester (5.9 g, 20 mmol) in ethanol (100 mL) and the resulting mixture was heated at reflux for 2 hours. The reaction mixture was then cooled and concentrated under reduced pressure. The residue was acidified until pH 3 ca. by addition of an aqueous solution of hydrochloric acid. The resulting mixture was extracted twice with dichloromethane and the combined organic extracts were dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure to give 5.329 g of 7-bromo-3-methoxy-naphthalene-2-carboxylic acid as a cream colored solid.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 2 hours
  3. temperatureThe reaction mixture was then cooled
  4. concentrationconcentrated under reduced pressure
  5. additionThe residue was acidified until pH 3 ca. by addition of an aqueous solution of hydrochloric acid
  6. extractionThe resulting mixture was extracted twice with dichloromethane
  7. dry with materialthe combined organic extracts were dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. customevaporated under reduced pressure