反応 #2253

反応方程式

N-(3-chloro-phenyl)-4-(N-oxido-4-pyridyl)-2-pyrimidineamine

phosphorus oxychloride

sodium hydroxide

→

N-(3-chloro-phenyl)-4-(2-chloro4-pyridyl)-2-pyrimidineamine

反応条件

後処理

1. 1
   抽出extracted with tetrahydrofuran
2. 2
   濃縮Concentration and crystallisation (tetrahydrofuran/ethanol) of the residue

実験手順

10.0 g (32 mmol) of N-(3-chloro-phenyl)-4-(N-oxido-4-pyridyl)-2-pyrimidineamine are stirred for 24 h in 100 ml of phosphorus oxychloride at 110°. The reaction mixture is stirred at 50° into 2N sodium hydroxide solution and extracted with tetrahydrofuran. Concentration and crystallisation (tetrahydrofuran/ethanol) of the residue give N-(3-chloro-phenyl)-4-(2-chloro4-pyridyl)-2-pyrimidineamine; m.p. 196°-198°, Rf =0.7 (methylene chloride:methanol=95:5).

出典