Sodium Iodide → HCID 178418729、化合物

HRID 432774

反応式

HRID 432774 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.[NH2:11][C:12]1[CH:16]=[C:15]([CH3:17])[NH:14][N:13]=1.C(N(C(C)C)CC)(C)C.[I-].[Na+]>C(O)CCC>[Cl:8][C:6]1[N:5]=[C:4]([S:9][CH3:10])[N:3]=[C:2]([NH:11][C:12]2[NH:13][N:14]=[C:15]([CH3:17])[CH:16]=2)[CH:7]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 805314,6-Dichloro-2-(methylthio)pyrimidineHCID 81531DiisopropylethylamineHCID 931461H-Pyrazol-3-amine, 5-methyl-

生成物 1

HCID 178418729HCID 178418729、化合物

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
120 °C

実験手順

To a solution of 4,6-dichloro-2-methylsulfanyl-pyrimidine (5 g, 25.6 mmol) and 3-amino-5-methylpyrazole 2.61 g, 26.9 mmol) in BuOH (60 mL) is added diisopropylethylamine (4.69 mL, 26.9 mmol) followed by sodium iodide (3.84 g, 25.6 mmol). The reaction mixture is stirred for 15 hours at 120° C. The solvent is then removed in vacuo and the residue is purified by flash chromatography (SiO2, hexane/AcOEt gradient) to give [6-chloro-2-methylsulfanyl-pyrimidin-4-yl)-(5-methyl-2H-pyrazol-3-yl)-amine.

後処理

  1. customThe solvent is then removed in vacuo
  2. customthe residue is purified by flash chromatography (SiO2, hexane/AcOEt gradient)

出典と根拠

ORDレコード
ord-43ee8d04ab434e169325ab201a997d28
出典データセット
uspto-grants-2003_12
特許番号
US06664247B2

関連ノート

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