反応 #56933

反応方程式

2-(2-amino-6-chloro-pyrimidin-4-yl)-4-bromo-phenol

1-bromomethyl-4-nitro-benzene

cesium carbonate

hydrogen chloride

dioxane

→

6-[5-bromo-2-(4-nitro-benzyloxy)-phenyl]-6-chloro-pyrimidin-2-ylamine

溶媒

acetonitrile

ethyl acetate

反応条件

後処理

1. 1
   ろ過Filtration and concentration of the filtrate
2. 2
   その他provided a crude product which
3. 3
   workup.ADDITIONwas added
4. 4
   ろ過Filtration

実験手順

A stirred suspension of 2-(2-amino-6-chloro-pyrimidin-4-yl)-4-bromo-phenol (0.151 g, 0.50 mmol), 1-bromomethyl-4-nitro-benzene (0.218 g, 1.0 mmol), and cesium carbonate (0.325 g, 1.0 mmol) in acetonitrile (10 ml) was stirred at 80° C. for 2 hours. Filtration and concentration of the filtrate provided a crude product which was dissolved in ethyl acetate (10 ml) and stirred while a 4 M solution of hydrogen chloride in dioxane (0.50 ml, 2.0 mmol) was added. Filtration provided 6-[5-bromo-2-(4-nitro-benzyloxy)-phenyl]-6-chloro-pyrimidin-2-ylamine as hydrochloride salt (0.23 g, 96% yield).

出典