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Methyl iodide → HCID 23078267、化合物

HRID 228801
ノート
印刷プレビュー

反応式

HRID 228801 の反応式
[F:1][C:2]1[N:7]=[C:6]([I:8])[C:5]([OH:9])=[CH:4][CH:3]=1.CI.[C:12](=O)([O-])[O-].[K+].[K+]>C(#N)C>[F:1][C:2]1[N:7]=[C:6]([I:8])[C:5]([O:9][CH3:12])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 195976736-Fluoro-2-iodopyridin-3-ol

生成物 1

HCID 23078267HCID 23078267、化合物収率 100%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

6-Fluoro-2-iodo-pyridin-3-ol (50 mg) was dissolved in acetonitrile (2 ml) to prepare a solution. Methyl iodide (148 mg) and potassium carbonate (87 mg) were added to the solution, and the mixture was stirred at room temperature overnight. The solvent was removed by distillation under the reduced pressure, water was then added to the residue, and the mixture was extracted with chloroform. The chloroform layer was washed with water and was dried over anhydrous magnesium sulfate, the solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform to give 6-fluoro-2-iodo-3-methoxypyridine (52 mg, yield 100%).

後処理

  1. customto prepare a solution
  2. customThe solvent was removed by distillation under the reduced pressure, water
  3. additionwas then added to the residue
  4. extractionthe mixture was extracted with chloroform
  5. washThe chloroform layer was washed with water
  6. dry with materialwas dried over anhydrous magnesium sulfate
  7. customthe solvent was removed by distillation under the reduced pressure
  8. customthe residue was purified by thin layer chromatography

出典と根拠

ORDレコード
ord-5a4a2009f657482682cbaf6a43b28d3e
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07560558B2

反応ノート

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