HRID973537

反应详情

EQUATION

反应方程式

HRID 973537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 1 l of methanol was dissolved 180 g of monomethyl terephthalate, and the solution was slowly added dropwise to 500 ml of hydrazine hydrate (50%) at room temperature while stirring. After the drop-wise addition, the mixture was heat-refluxed for 5 hours while stirring. A hydrochloric acid aqueous solution was slowly added to the reaction mixture to adjust to a pH of about 1 to thereby precipitate white crystals. Two liters of water was added to the system, followed by stirring for a while. The formed crystals were collected by filtration under reduced pressure, washed twice with 200 ml of water, and dried to obtain 160 g of p-carboxybenzhydrazide (melting point: 235-236° C.).

WORKUP

后处理

  1. additionAfter the drop-wise addition
  2. temperaturethe mixture was heat-refluxed for 5 hours
  3. stirringwhile stirring
  4. customto thereby precipitate white crystals
  5. additionTwo liters of water was added to the system
  6. stirringby stirring for a while
  7. filtrationThe formed crystals were collected by filtration under reduced pressure
  8. washwashed twice with 200 ml of water
  9. customdried