Methyl iodide → N-(2-Chloro-4-pyrimidinyl)-N,2,3-trimethyl-2H-indazol-6-amine

HRID 1801850ノート

反応式

HRID 1801850 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:10]=[CH:11][C:12]3[C:16]([CH:17]=2)=[N:15][N:14]([CH3:18])[C:13]=3[CH3:19])[CH:5]=[CH:4][N:3]=1.[C:20](=O)([O-])[O-].[Cs+].[Cs+].IC>CN(C=O)C>[Cl:1][C:2]1[N:7]=[C:6]([N:8]([CH3:20])[C:9]2[CH:10]=[CH:11][C:12]3[C:16]([CH:17]=2)=[N:15][N:14]([CH3:18])[C:13]=3[CH3:19])[CH:5]=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 11637631N-(2-Chloro-4-pyrimidinyl)-2,3-dimethyl-2H-indazol-6-amine

生成物 1

HCID 11608962N-(2-Chloro-4-pyrimidinyl)-N,2,3-trimethyl-2H-indazol-6-amine収率 37%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-(2-chloropyrimidin-4-yl)-2,3-dimethyl-2H-indazol-6-amine (2.21 g; 8 mmol, 1 equiv) was dissolved in DMF (11 ml) and cesium carbonate (7.9 g; 24.2 mmol, 3 equiv) was added. The reaction mixture was stirred for 30 min under nitrogen. Iodomethane (0.8 ml, 13 mmol, 1.6 equiv) was added and the reaction mixture was stirred at room temperature for 2 hrs. The reaction mixture was poured in ice cold water and stirred for 30 minutes. The resulting precipitate was collected by filtration to yield the desired compound (0.84 g, 37%).

後処理

  1. stirringthe reaction mixture was stirred at room temperature for 2 hrs
  2. additionThe reaction mixture was poured in ice cold water
  3. stirringstirred for 30 minutes
  4. filtrationThe resulting precipitate was collected by filtration

出典と根拠

ORDレコード
ord-2a481b647c3c45d780f7e2948ea83963
出典データセット
uspto-grants-2013_01
特許番号
US08349861B2

反応ノート

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