Methyl iodide → HCID 67653887、化合物

HRID 2393339ノート

反応式

HRID 2393339 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([CH2:9][C:10]([O:12][CH3:13])=[O:11])=[C:4]([O:14][C:15]2[CH:16]=[N:17][N:18]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[CH3:26])[CH:19]=2)[N:3]=1.[H-].[Na+].C(CNC[CH:34]=[O:35])=O.[CH3:36]I>CN(C)C=O.COCCOC>[CH3:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([C:9](=[CH:36][O:35][CH3:34])[C:10]([O:12][CH3:13])=[O:11])=[C:4]([O:14][C:15]2[CH:16]=[N:17][N:18]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[CH3:26])[CH:19]=2)[N:3]=1

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 18975607HCID 18975607、化合物HCID 202686642,2'-Azanediyldiacetaldehyde

生成物 1

HCID 67653887HCID 67653887、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
45 °C

実験手順

The intermediate methyl 2-[2,4-dimethyl-6-(1-(2-methylphenyl)-1H-pyrazol-4-yloxy)-pyrimidin-5-yl]-acetate (6.0 g, 17 mmol), sodium hydride (0.9 g, 37 mmol) and N,N-diformylmethylamine (6 ml) in a mixture of dimethylformamide (20 ml) and 1,2-dimethoxyethane (20 ml) is stirred at 45° C. for 3 hours. Methyliodide (4.2 g, 30 mmol) is added at room temperature and stirring is continued for additional 16 hours. Dilution with ether, washing with brine, drying and chromatography on silicagel (eluant ethyl acetate/hexane 3:7) gives methyl 2-[2,4-dimethyl-6-(1-(2-methylphenyl)-1H-pyrazole-4-yloxy)-pyrimidin-5-yl]-3-methoxyacrylate as a colorless oil.

後処理

  1. stirringstirring
  2. waitis continued for additional 16 hours
  3. washDilution with ether, washing with brine
  4. customdrying

出典と根拠

ORDレコード
ord-4a4730f52f544326813c7b8d75189987
出典データセット
uspto-grants-1998_09
特許番号
US05807863

反応ノート

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