HRID358875

反应详情

EQUATION

反应方程式

HRID 358875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5 ml of concentrated sulfuric acid and 1.2 ml of water were added to 1.24 g (0.007 mole) of 3-methoxy-2,4,5-trifluorobenzonitrile (XXIV) [prepared as described in Step (E4) above], and the mixture was heated at 100°-140° C. for 30 minutes, poured into ice-water, and extracted with ethyl acetate. The extract was washed with water and dried, and the solvent was removed by evaporation under reduced pressure to afford 1.10 g of 3-methoxy-2,4,5-trifluorobenzamide (XXV) as a pale brown powder melting at 131°-133° C.

WORKUP

后处理

  1. temperaturethe mixture was heated at 100°-140° C. for 30 minutes
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water
  4. customdried
  5. customthe solvent was removed by evaporation under reduced pressure