Trifluoroacetic acid → 2-[(2,5-Dichloropyridin-3-yl)oxy]-2-methylpropionic acid

HRID 1026539ノート

反応式

HRID 1026539 の反応式
[Cl:1][C:2]1[C:7]([O:8][C:9]([CH3:18])([CH3:17])[C:10]([O:12]C(C)(C)C)=[O:11])=[CH:6][C:5]([Cl:19])=[CH:4][N:3]=1.FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:7]([O:8][C:9]([CH3:17])([CH3:18])[C:10]([OH:12])=[O:11])=[CH:6][C:5]([Cl:19])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86671386Tert-butyl 2-[(2,5-dichloropyridin-3-yl)oxy]-2-methylpropionate

生成物 1

HCID 866713872-[(2,5-Dichloropyridin-3-yl)oxy]-2-methylpropionic acid収率 125.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a dichloromethane solution (157 ml) of tert-butyl 2-[(2,5-dichloropyridin-3-yl)oxy]-2-methylpropionate (79.1 g) was added at 0° C. trifluoroacetic acid (157 ml). The reaction solution was brought back to room temperature, stirred overnight, and then concentrated under reduced pressure. The residue was dissolved in ethyl acetate, washed sequentially with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was azeotroped with toluene to afford 2-[(2,5-dichloropyridin-3-yl)oxy]-2-methylpropionic acid (81.1 g).

後処理

  1. customwas brought back to room temperature
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed sequentially with water and saturated sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was azeotroped with toluene

出典と根拠

ORDレコード
ord-0b56ff09ed5144dda50816a792bad4d0
出典データセット
uspto-grants-2014_05
特許番号
US08729095B2

反応ノート

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