Water → 5-Iodo-N,N-dimethylpyridin-2-amine

HRID 454809

反応式

HRID 454809 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][C:6]([I:9])=[CH:5][N:4]=1.[C:10](=O)([O-])[O-].[K+].[K+].IC.O>CC(N(C)C)=O>[CH3:1][N:2]([C:3]1[CH:8]=[CH:7][C:6]([I:9])=[CH:5][N:4]=1)[CH3:10]

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 11253290(5-Iodo-pyridin-2-yl)-methyl-amine

生成物 1

HCID 234385795-Iodo-N,N-dimethylpyridin-2-amine収率 57%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
90 °C

実験手順

The obtained 2-(N-monomethylamino)-5-iodopyridine (99, 1.00 g, 4.27 mmol), potassium carbonate (2.95 g, 21.36 mmol) and iodomethane (145 mg, 8.546 mmol) were dissolved in dimethylacetamide (30 mL), and the reaction mixture was heated at 90° C. for 24 hours, followed by adding water. Organic compounds were extracted with ethyl acetate and evaporated after a treatment with sodium sulfate. Purification was performed by column chromatograph to give the target compound 2-(N,N-dimethylamino)-5-iodopyridine (100, 603 mg, 57%).

後処理

  1. extractionOrganic compounds were extracted with ethyl acetate
  2. customevaporated after a treatment with sodium sulfate
  3. customPurification

出典と根拠

ORDレコード
ord-f7704ee6c4784f8ab3530aa48939cf40
出典データセット
uspto-grants-2013_07
特許番号
US08497260B2

関連ノート

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