Water → [1-(6-Amino-pyrimidin-4-yl)-1H-benzoimidazol-2-yl]-(2-methyl-5-nitro-phenyl)-amine

HRID 1968423

反応式

HRID 1968423 の反応式
Cl[C:2]1[N:6]([C:7]2[N:12]=[CH:11][N:10]=[C:9]([NH2:13])[CH:8]=2)[C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=2[N:3]=1.C[C:19]1C=[C:23]([N+:25]([O-:27])=[O:26])[CH:22]=[CH:21][C:20]=1N.CS(O)(=O)=O.O.C[N:36]1[CH2:40][CH2:39]N(C)C1=O>>[NH2:13][C:9]1[N:10]=[CH:11][N:12]=[C:7]([N:6]2[C:5]3[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=3[N:3]=[C:2]2[NH:36][C:40]2[CH:39]=[C:23]([N+:25]([O-:27])=[O:26])[CH:22]=[CH:21][C:20]=2[CH3:19])[CH:8]=1

参加物

6

反応物 5

HCID 962WaterHCID 6395Methanesulfonic AcidHCID 66611,3-Dimethyl-2-imidazolidinoneHCID 74412-Methyl-4-nitroanilineHCID 598224556-(2-Chloro-1H-benzimidazol-1-yl)pyrimidin-4-amine

生成物 1

HCID 15949047[1-(6-Amino-pyrimidin-4-yl)-1H-benzoimidazol-2-yl]-(2-methyl-5-nitro-phenyl)-amine

実験手順

A solution of 6-(2-chloro-benzoimidazol-1-yl)-pyrimidin-4-ylamine (110 mg, 0.45 mmol), 2-methyl-4-nitro-phenylamine (103 mg, 0.68 mmol), and MeSO3H (58.0 μL, 0.9 mmol) in 1,3-dimethyl-2-imidazolidinone (0.2 ml) is heated at 90° C. After stirring for 2 hours, the reaction mixture is cooled to room temperature and is treated with water (5 mL). Solid is collected via filtration and further purified by flash chromatography on silica gel (0% MeOH/Dichloromethane to 10% MeOH/Dichloromethane gradient). The title compound is obtained as white powder.

後処理

  1. filtrationSolid is collected via filtration
  2. customfurther purified by flash chromatography on silica gel (0% MeOH/Dichloromethane to 10% MeOH/Dichloromethane gradient)

出典と根拠

ORDレコード
ord-d16c29f5fe4a438bad1e80d39fea7ea1
出典データセット
uspto-grants-2013_04
特許番号
US08426404B2

関連ノート

読み込み中…