Sodium Hydroxide → N-(3-chlorophenyl)-4-(2-chloropyridin-4-yl)pyrimidin-2-amine

HRID 2157

反応式

HRID 2157 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[N:14]=[C:13]([C:15]3[CH:20]=[CH:19][N+:18]([O-])=[CH:17][CH:16]=3)[CH:12]=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1.[OH-].[Na+].P(Cl)(Cl)([Cl:26])=O>>[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[N:14]=[C:13]([C:15]3[CH:20]=[CH:19][N:18]=[C:17]([Cl:26])[CH:16]=3)[CH:12]=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 19689585N-(3-chloro-phenyl)-4-(N-oxido4-pyridyl)-2-pyrimidineamine

生成物 1

HCID 9905031N-(3-chlorophenyl)-4-(2-chloropyridin-4-yl)pyrimidin-2-amine

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).

後処理

  1. extractionextracted with tetrahydrofuran
  2. concentrationConcentration and crystallisation (tetrahydrofuran/ethanol) of the residue

出典と根拠

ORDレコード
ord-d187a558f2cb415e8f8f2e8cc58499db
出典データセット
uspto-grants-1998_03
特許番号
US05728708

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