反応式
[NH2:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([O:8][CH2:9][CH2:10][OH:11])[C:3]=1[C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=1.[H-].[Na+].[Br:21][C:22]1[CH:23]=[N:24][C:25](Cl)=[N:26][CH:27]=1.[Cl-].[NH4+]>O1CCCC1>[Br:21][C:22]1[CH:23]=[N:24][C:25]([O:11][CH2:10][CH2:9][O:8][C:4]2[N:5]=[CH:6][N:7]=[C:2]([NH2:1])[C:3]=2[C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)=[N:26][CH:27]=1参加物
実験手順
To a solution of 2-{6-amino-5-(4-methylphenyl)pyrimidin-4-yloxy}-ethanol (7.54 g) in tetrahydrofuran (150 ml) is added sodium hydride (60% dispersion-type, 1.47 g), and thereto is added 5-bromo-2-chloropyrimidine (7.73 g), and the mixture is stirred at room temperature overnight. To the reaction solution is added saturated aqueous ammonium chloride solution, and the mixture is evaporated to remove the solvent. The precipitated crystals are collected by filtration, washed and dried. The crude crystals are purified by silica gel column chromatography (solvent; chloroform/methanol=100:1~80:1), and recrystallized from tetrahydrofuran/diethyl ether to give 6-[2-(5-bromopyrimidin-2-yloxy)ethoxy]-5-(4-methylphenyl)pyrimidin-4-amine (11.27 g).
後処理
- customthe mixture is evaporated
- customto remove the solvent
- filtrationThe precipitated crystals are collected by filtration
- washwashed
- customdried
- customThe crude crystals are purified by silica gel column chromatography (solvent; chloroform/methanol=100:1~80:1)
- customrecrystallized from tetrahydrofuran/diethyl ether
出典と根拠
- ORDレコード
- ord-a7b7ef5f674140eda2b87b65e3637f7d
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05728706
関連ノート
読み込み中…