HRID1382131

反应详情

EQUATION

反应方程式

HRID 1382131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 1000 ml round-bottomed flask equipped with a stirrer, thermometer and Marcusson-condenser 180 g (3 moles) of n-propanol, and 380 g of benzene are weighed in, whereupon 493 g (2 moles) of 4-chloro-3,5-dinitro-benzoic acid and 20 g of concentrated sulfuric acid are added under stirring. The reaction mixture is heated to boiling on a water bath under stirring (86° C.) until no more water is distilled off. The water thus formed is collected in the Marcusson-condenser and removed if necessary. In the meantime the upper benzene/n-propanol phase is continuously re-introduced into the flask. The reaction having been completed the mixture is cooled to room temperature under stirring, the precipitated crystals are filtered off, washed with cold n-propanol and dried. Thus 490 g of the desired compound are obtained, yield 85%, purity 98%.

WORKUP

后处理

  1. customInto a 1000 ml round-bottomed flask equipped with a stirrer
  2. temperatureThe reaction mixture is heated
  3. customto boiling on a water bath
  4. distillationis distilled off
  5. customThe water thus formed
  6. customis collected in the Marcusson-condenser
  7. customremoved if necessary
  8. additionIn the meantime the upper benzene/n-propanol phase is continuously re-introduced into the flask
  9. stirringunder stirring
  10. filtrationthe precipitated crystals are filtered off
  11. washwashed with cold n-propanol
  12. customdried