HRID2239840
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
CONDITIONS
反应条件
- 温度
- 118 °C
PROCEDURE
实验过程
Chloroacetaldehyde (2.0 mL, 31.5 mmol) was added to a solution of crude 4-bromo-6-chloro-5-phenylpyridazin-3-amine (0.193 g, 0.676 mmol) from 1b in EtOH (5.0 mL). The mixture was heated in a sealed tube at 118° C. for 5 h. After cooling to room temperature, the reaction mixture was concentrated in vacuo, and suspended in acetone/Et2O (1:1, 3 mL), filtered, and washed with Et2O to give 8-bromo-6-chloro-7-phenylimidazo[1,2-b]pyridazine HCl salt (0.147 g, >94% purity).
WORKUP
后处理
- temperatureAfter cooling to room temperature
- concentrationthe reaction mixture was concentrated in vacuo
- filtrationfiltered
- washwashed with Et2O