HRID379082

反应详情

EQUATION

反应方程式

HRID 379082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium carbonate (13.8 g) is added to a solution of 1,2-dichloro-3-nitrobenzene (19.29 g) and 2,4-dichlorothio-phenol (17.9 g) in xylene (250 ml), and the resulting mixture is heated for 5 hours at reflux temperature. The precipitate is separated by filtration, washed with xylene and the combined organic phases are concentrated. The resultant residue is mixed with petroleum ether and stirred for 1 hour at room temperature. Following this, the crystalline material is suction filtered and washed with petroleum ether, and any remaining solvent is removed in a vacuum. Yield: 25.6 g of colourless crystals (76.6%).

WORKUP

后处理

  1. temperaturethe resulting mixture is heated for 5 hours
  2. temperatureat reflux temperature
  3. customThe precipitate is separated by filtration
  4. washwashed with xylene
  5. concentrationthe combined organic phases are concentrated
  6. additionThe resultant residue is mixed with petroleum ether
  7. filtrationfiltered
  8. washwashed with petroleum ether
  9. customany remaining solvent is removed in a vacuum