HRID442262

反应详情

EQUATION

反应方程式

HRID 442262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.2 grams of 2-fluoro-5-nitroaniline, sulfuric acid (3 cc., d 1.84) and 8 ml. of water is stirred into a solution of 1.5 grams of sodium nitrite in water, maintained below 5° C. After 10 minutes, the excess nitrous acid is destroyed by urea, the reaction mixture filtered, and the filtrate added to 40 ml. of boiling 50% sulfuric acid. After complete addition, the mixture is boiled an additional 15 minutes, cooled, and the separated phenol filtered and washed with water. It is then purified by recrystallization from hexane.

WORKUP

后处理

  1. temperaturemaintained below 5° C
  2. customthe excess nitrous acid is destroyed by urea
  3. filtrationthe reaction mixture filtered
  4. additionthe filtrate added to 40 ml
  5. additionAfter complete addition
  6. waitthe mixture is boiled an additional 15 minutes
  7. temperaturecooled
  8. filtrationthe separated phenol filtered
  9. washwashed with water
  10. customIt is then purified by recrystallization from hexane