HRID465156

反应详情

EQUATION

反应方程式

HRID 465156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.5 kg (10 mol) hydrazine hydrate was heated with 3.040 kg (20 mol) salicylic acid methyl ester and 2.714 kg vaseline in a protective gas such as nitrogen or argon in the apparatus according to the invention. The water-methanol mixture produced was continuously distilled-off from the reaction mixture. After about three hours, the reaction temperature had risen to 120° C. and approximately half of the quantity of methanol expected theoretically and the entire amount of water were distilled off (0.5 kg). The hydrazide was present in the vaseline as a crystal product in paste. The heating was continued after 30 g boron trioxide was added and the temperature was kept at 150° C. The remaining methanol (0.320 kg) was distilled off. After about three hours, the reaction was complete as determined by the amount of methanol distilled off.

WORKUP

后处理

  1. customhad risen to 120° C.
  2. distillationthe entire amount of water were distilled off (0.5 kg)
  3. additionwas added
  4. customwas kept at 150° C
  5. distillationThe remaining methanol (0.320 kg) was distilled off
  6. waitAfter about three hours
  7. distillationdistilled off