Dimethylformamide → 3-(2-Fluoro-4-nitrophenoxy)pyridine

HRID 13233

反応式

HRID 13233 の反応式
[OH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.[F:19][C:20]1[CH:21]=[C:22]([N+:27]([O-:29])=[O:28])[CH:23]=[CH:24][C:25]=1F>C(OCC)(=O)C>[F:19][C:20]1[CH:21]=[C:22]([N+:27]([O-:29])=[O:28])[CH:23]=[CH:24][C:25]=1[O:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 79713-HydroxypyridineHCID 11430Potassium CarbonateHCID 1230531,2-Difluoro-4-nitrobenzene

生成物 1

HCID 231451003-(2-Fluoro-4-nitrophenoxy)pyridine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

2.09 g of 3-hydroxypyridine and 5.52 g of potassium carbonate were added to a dimethylformamide (20 ml) solution of 3.18 g of 3,4-difluoronitrobenzene, and the reaction liquid was stirred at 90° C. for 1 hour. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=9/1) to obtain the entitled compound.

後処理

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with water and saturated saline in order
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=9/1)
  7. customto obtain the entitled compound

出典と根拠

ORDレコード
ord-ae345408704b4fb4b3c1225ccec86d21
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

関連ノート

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