HRID265666

反应详情

EQUATION

反应方程式

HRID 265666 的结构方程式

PROCEDURE

实验过程

Into a 100 ml glass reactor equipped with a reflux condenser, a stirrer and a dropping funnel, 20 ml of a methanol solution of 10 g (0.0397 mol) of the 3,4,5,6-tetrafluorophthalic acid-monomethyl ester prepared in Example 14 was charged, and then 4.6 g (0.083 mol) of potassium hydroxide was added thereto. The mixture was stirred for one hour under reflux. After completion of the reaction, the reaction mixture was neutralized with a 10% of hydrochloric acid aqueous solution and extracted with ethyl acetate. Then, the solvent was distilled off to obtain 8.2 g of 4-methoxy-3,5,6-trifluorophthalic acid-1-methyl ester. (=5-methoxy-3,4,6-trifluorophthalic acid-2-methyl ester.) The yield was 78.2%.

WORKUP

后处理

  1. customInto a 100 ml glass reactor equipped with a reflux condenser, a stirrer and a dropping funnel
  2. temperatureunder reflux
  3. customAfter completion of the reaction
  4. extractionextracted with ethyl acetate
  5. distillationThen, the solvent was distilled off