Potassium Iodide → N-(2,6-difluoropyridin-3-yl)-N-(2-oxopropyl)formamide

HRID 546781ノート

反応式

HRID 546781 の反応式
Cl[CH2:2][C:3](=[O:5])[CH3:4].C(=O)([O-])[O-].[Cs+].[Cs+].[I-].[K+].[F:14][C:15]1[C:20]([NH:21][CH:22]=[O:23])=[CH:19][CH:18]=[C:17]([F:24])[N:16]=1>CN(C)C=O.O.C(OCC)(=O)C>[F:14][C:15]1[C:20]([N:21]([CH2:2][C:3](=[O:5])[CH3:4])[CH:22]=[O:23])=[CH:19][CH:18]=[C:17]([F:24])[N:16]=1

参加物

8

反応物 4

HCID 4875Potassium IodideHCID 6571ChloroacetoneHCID 10796Cesium carbonateHCID 86628515N-(2,6-difluoropyridin-3-yl)formamide

生成物 1

HCID 86628516N-(2,6-difluoropyridin-3-yl)-N-(2-oxopropyl)formamide

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Chloroacetone (1.83 ml), cesium carbonate (7.99 g) and potassium iodide (254 mg) were added to a solution of N-(2,6-difluoropyridin-3-yl)formamide (2.42 g) in N,N-dimethylformamide (50 ml), and the reaction solution was stirred at room temperature for two hours. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and then the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (2.52 g). The property values of the compound are as follows.

後処理

  1. customthe organic layer was separated
  2. washThe resulting organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe drying agent was separated by filtration
  5. concentrationthe organic layer was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-cfc561bdf5c74c69baf3294907009449
出典データセット
uspto-grants-2011_05
特許番号
US07935815B2

反応ノート

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