HRID1709957

反应详情

EQUATION

反应方程式

HRID 1709957 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

59 g of hydrazine hydrate was dissolved in 712 ml of acetonitrile at room temperature under an atmosphere of nitrogen. A solution obtained by dissolving 46.3 g of 1,2-dichloro-4-nitrobenzene in 71 g of acetonitrile was added dropwisely to the obtained solution. After the addition had been completed, the obtained mixture was subjected to reflux by heat for 4 hours, and the reaction solution was concentrated. 500 g of water was added to the concentrate, and the produced crystals were filtered off. 200 g of acetonitrile was then added to the crystals, and the obtained mixture was subjected to reflux by heat for 30 minutes and then cooled with ice to room temperature. The produced crystals were filtered off (yield: 27 g).

WORKUP

后处理

  1. customA solution obtained
  2. additionwas added dropwisely to the obtained solution
  3. additionAfter the addition
  4. temperatureto reflux
  5. temperatureby heat for 4 hours
  6. concentrationthe reaction solution was concentrated
  7. addition500 g of water was added to the concentrate
  8. filtrationthe produced crystals were filtered off
  9. addition200 g of acetonitrile was then added to the crystals
  10. temperatureto reflux
  11. temperatureby heat for 30 minutes
  12. filtrationThe produced crystals were filtered off (yield: 27 g)