HRID462408
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionA mixture of 2.69 g
- temperatureat reflux for 16 hours
- temperaturecooled
- filtrationfiltered
- customgiving an orange solid which
- temperatureThe filtrate is heated
- temperatureat reflux for 23 hours
- temperaturechilled in an ice bath
- filtrationfiltered
- customgiving more orange solid
- customrecrystallized from dimethylformamide
- customgiving 0.65 g