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Dimethylformamide → HCID 22494013、化合物

HRID 1816656
ノート
印刷プレビュー

反応式

HRID 1816656 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4](O)[CH:3]=1.[CH2:12](I)[CH3:13].[C:15](=O)([O-])[O-].[K+].[K+].CN(C)[CH:23]=[O:24]>O>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH2:12][CH3:13])=[O:7])=[C:4]([O:24][CH2:23][CH3:15])[CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 787824-Chlorosalicylic acid

生成物 1

HCID 22494013HCID 22494013、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

5.0 g of 4-chloro-2-hydroxybenzoic acid was dissolved in 25 ml dimethylformamide, and 14.5 g of ethyl iodide and 12 g of potassium carbonate were added thereto, followed by stirring at 70° C. for 8 hours. The reaction solution was diluted with water and then extracted with ethyl acetate. The organic layer was successively washed with 1N hydrochloric acid and brine, dried over anhydrous magnesium sulfate and the solvent was evaporated. The residue was subjected to silica gel column chromatography, and from fractions eluted with hexane-ethyl acetate (2:1), 3.8 g of ethyl 4-chloro-2-ethoxybenzoate was obtained.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was successively washed with 1N hydrochloric acid and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated
  5. washfrom fractions eluted with hexane-ethyl acetate (2:1)

出典と根拠

ORDレコード
ord-13672613756e4ca7a67eedb6eda20735
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06884821B1

反応ノート

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