HRID2192376

反应详情

EQUATION

反应方程式

HRID 2192376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customquenched with H2O (1.5 mL)
  2. stirringstirred for 20 mins
  3. concentrationbefore concentrating under reduced pressure to a brown solid
  4. customThe crude product was purified by silica gel chromatography
  5. washeluting with 1-2% MeOH/dichloromethane
  6. customevaporated