HRID328286

反应详情

EQUATION

反应方程式

HRID 328286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 2-cyano-4-trifluoromethyl-benzoate (102.3 g.), sodium hydroxide pellets (108 g.), water (900 cc.) and methanol (1,900 cc.) are heated to the reflux temperature for 12 hours. The solution is decolorised by means of animal charcoal (0.6 g.). After filtration, hydrochloric acid (d = 1.19) (100 cc.) is added. The mixture is extracted with ethyl ether (2.25 liters). The organic layer is dried over anhydrous magnesium sulphate (40 g.). After filtering, and concentrating the filtrate, 4-trifluoromethyl-phthalic acid (99.1 g.) melting at 178° C is obtained.

WORKUP

后处理

  1. filtrationAfter filtration, hydrochloric acid (d = 1.19) (100 cc.)
  2. additionis added
  3. extractionThe mixture is extracted with ethyl ether (2.25 liters)
  4. dry with materialThe organic layer is dried over anhydrous magnesium sulphate (40 g.)
  5. filtrationAfter filtering
  6. concentrationconcentrating the filtrate