HRID596753

反应详情

EQUATION

反应方程式

HRID 596753 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

35.4 g of oxalic acid bis-hydrazide are suspended in 1000 ml of dimethyl acetamide, the suspension is briefly heated to 100° C and cooled to room temperature, and 93.5 g of salicylic acid chloride are slowly added in such a way that the reaction temperature does not exceed 40° C. After a further 15 minutes' stirring a largely homogeneous, yellowish solution has been obtained. After filtering off the undissolved constituents, the solution is mixed with 1.2 liters of ice water, whereupon the reaction product precipitates. The substance is filtered off, washed with water and purified by again precipitating it from dimethyl acetamide solution by means of water. After isolation and intensive drying at 130° C in vacuo, N,N'-bis-(salicyloyl)-oxalic acid dihydrazide (Stabiliser No. 2) is obtained as a white powder of melting point>320° C (decomposition).

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. customdoes not exceed 40° C
  3. customhas been obtained
  4. filtrationAfter filtering off the undissolved constituents
  5. additionthe solution is mixed with 1.2 liters of ice water, whereupon the reaction product
  6. customprecipitates
  7. filtrationThe substance is filtered off
  8. washwashed with water
  9. custompurified
  10. customby again precipitating it from dimethyl acetamide solution by means of water
  11. customAfter isolation and intensive drying at 130° C in vacuo