HRID1813870

反应详情

EQUATION

反应方程式

HRID 1813870 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 400 ml of water, 21.7 g of bromosalicylic acid, 13.41 g of phenyl borate and 15.28 g of potassium carbonate were dissolved. The solution was stirred at room temperature for 40 minutes. The completion of the reaction was confirmed by TLC, and the reaction solution was poured into a mixture of diluted hydrochloric acid and ethyl acetate. The organic phase was extracted, separated, and washed with a saturated aqueous sodium chloride solution. The organic phase was dried with magnesium sulfate, and concentrated. The concentrate was recrystallized with acetonitrile to obtain 5-phenylsalicyclic acid as colorless crystals. The amount was 18.58 g (yield: 87%). The molecular structure was confirmed with a mass spectrum. Synthesis of ethyl 5-phenylsalicylate

WORKUP

后处理

  1. extractionThe organic phase was extracted
  2. customseparated
  3. washwashed with a saturated aqueous sodium chloride solution
  4. dry with materialThe organic phase was dried with magnesium sulfate
  5. concentrationconcentrated
  6. customThe concentrate was recrystallized with acetonitrile