HRID1356662

反应详情

EQUATION

反应方程式

HRID 1356662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a suspension of 4′-fluoro-p-toluenesulfonanilide (486.6 g (1.80 mol) in acetic acid (955 ml), 97% fuming nitric acid (128.6 g (1.98 mol) was added dropwise, keeping the inner temperature at 45° C., over a period of 40 minutes. After completion of the addition, the reaction mixture was stirred at 50° C. for 2 hours and left to cool to room temperature. Water (2000 ml) was then added and the mixture was stirred for 30 minutes. The crystals separated were filtered and washed with water to give 543.5 g (97%) of 4′-fluoro-2′-nitro-p-toluenesulfonanilide as yellow crystals.

WORKUP

后处理

  1. customat 45° C.
  2. additionAfter completion of the addition
  3. waitleft
  4. temperatureto cool to room temperature
  5. stirringthe mixture was stirred for 30 minutes
  6. customThe crystals separated
  7. filtrationwere filtered
  8. washwashed with water