HRID870695
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
- 100 °C
PROCEDURE
实验过程
A mixture of 3,6-dichloro-4-methylpyridazine (1.35 g, 8.28 mmol) and 2,4-dimethoxybenzylamine (11.1 g, 66.3 mmol) in i-PrOH (5 ml) was heated in a microwave at 100° C. for 50 min. (30+20 min.). The mixture was concentrated and the residue was subjected to ISCO (120 g column, hexane 5 min., 0-55% EtOAc in hexane over 90 min. to give (6-chloro-5-methyl-pyridazin-3-yl)-(2,4-dimethoxy-benzyl)-amine (680 mg) plus the 6-methyl analog (320 mg).
WORKUP
后处理
- concentrationThe mixture was concentrated
- custom120 g column, hexane 5 min., 0-55% EtOAc in hexane
- customover 90 min.