(2,4-Dichlorophenoxy)Acetic Acid → 2-(2,4-Dichlorophenoxy)ethanol

HRID 852060

反応式

HRID 852060 の反応式
[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:3]=1[O:4][CH2:5][C:6](O)=[O:7]>O1CCCC1>[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:3]=1[O:4][CH2:5][CH2:6][OH:7]

参加物

3

実験手順

To a solution of 2,4-dichlorophenoxy acetic acid (15.0 g) in tetrahydrofuran (300 mL) was added dropwise 1.0M borane-tetrahydrofuran complex/tetrahydrofuran solution (96 mL) under ice-cooling over 1.5 hours. The reaction solution was stirred at room temperature for 22 hours. After the reaction solution was concentrated, the residue was diluted with saturated aqueous ammonium chloride solution and ethyl acetate. The organic layer was washed with saturated ammonium chloride, saturated aqueous sodium hydrogencarbonate solution (×2) and saturated ammonium chloride, dried over anhydrous sodium sulfate and then concentrated, to give the title compound as a colorless oil (14 g).

後処理

  1. temperaturecooling over 1.5 hours
  2. concentrationAfter the reaction solution was concentrated
  3. additionthe residue was diluted with saturated aqueous ammonium chloride solution and ethyl acetate
  4. washThe organic layer was washed with saturated ammonium chloride, saturated aqueous sodium hydrogencarbonate solution (×2) and saturated ammonium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c770ce9aa5334bbaa74f3daed34a80bb
出典データセット
uspto-grants-2007_08
特許番号
US07253178B2

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