HRID34590

反应详情

EQUATION

反应方程式

HRID 34590 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

50 g of 3-fluoro-4-methyl-benzoic acid are initially introduced into 100 ml of concentrated sulphuric acid, and a mixture consisting of 26 g of 98% strength nitric acid and 40 g of concentrated sulphuric acid is added dropwise at 20°-25°, while cooling with ice. The mixture is subsequently stirred at room temperature for 1 hour. The batch is then poured onto ice-water and the crystals are filtered off with suction and washed thoroughly with water. After drying and recrystallization from toluene, 48 g (74.3% of theory) of 2-nitro-4-methyl-5-fluorobenzoic acid of melting point m.p.: 163°-5° C. are obtained.

WORKUP

后处理

  1. additionis added dropwise at 20°-25°
  2. temperaturewhile cooling with ice
  3. additionThe batch is then poured onto ice-water
  4. filtrationthe crystals are filtered off with suction
  5. washwashed thoroughly with water
  6. customAfter drying
  7. customrecrystallization from toluene, 48 g (74.3% of theory) of 2-nitro-4-methyl-5-fluorobenzoic acid
  8. customare obtained