HRID2192376
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 solution of bromoacetyl bromide (0.22 mL) in dry CHCl3 (4 mL) was added slowly to a suspension of 3-amino-6-methylpyridazine (0.24 g) and triethylamine (0.47 mL) in dry CHCl3 (45 mL) at room temperature. The brown mixture was allowed to stir for 3.5 hr, then quenched with H2O (1.5 mL) and stirred for 20 mins before concentrating under reduced pressure to a brown solid. The crude product was purified by silica gel chromatography eluting with 1-2% MeOH/dichloromethane. The relevant fractions were combined and evaporated to give the title compound (0.20 g) as a pinkish/beige solid.
WORKUP
后处理
- customquenched with H2O (1.5 mL)
- stirringstirred for 20 mins
- concentrationbefore concentrating under reduced pressure to a brown solid
- customThe crude product was purified by silica gel chromatography
- washeluting with 1-2% MeOH/dichloromethane
- customevaporated