HRID274588

反应详情

EQUATION

反应方程式

HRID 274588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixed solution of 2-nitro-4-methylbenzonitrile (15.8 g) in a mixture of 65% sulfuric acid and acetic acid (150 ml) was heated under reflux for 17 hours. After concentration, the residue was poured into ice-water and extracted with ethyl acetate. The extract was washed with water, dried and concentrated to dryness. Recrystallization of crystals from ether-hexane afforded colorless crystals (16.5 g, 94%), m.p. 156°-157° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 17 hours
  3. concentrationAfter concentration
  4. additionthe residue was poured into ice-water
  5. extractionextracted with ethyl acetate
  6. washThe extract was washed with water
  7. customdried
  8. concentrationconcentrated to dryness
  9. customRecrystallization of crystals from ether-hexane afforded colorless crystals (16.5 g, 94%), m.p. 156°-157° C.