HRID462408

反应详情

EQUATION

反应方程式

HRID 462408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.69 g. of 6-(p-bromophenyl)-3-chloropyridazine (U.S. Pat. No. 4,092,311), 3.12 g. of ethyl carbazate and 50 ml. of n-butanol is heated at reflux for 16 hours, then cooled and filtered giving an orange solid which is saved. The filtrate is heated at reflux for 23 hours, then chilled in an ice bath and filtered giving more orange solid. The two crops are combined and recrystallized from dimethylformamide, giving 0.65 g. of the desired product as orange crystals, m.p. 348°-350° C. (dec.).

WORKUP

后处理

  1. additionA mixture of 2.69 g
  2. temperatureat reflux for 16 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. customgiving an orange solid which
  6. temperatureThe filtrate is heated
  7. temperatureat reflux for 23 hours
  8. temperaturechilled in an ice bath
  9. filtrationfiltered
  10. customgiving more orange solid
  11. customrecrystallized from dimethylformamide
  12. customgiving 0.65 g