Water → 2-Hydroxydiphenyl ether

HRID 358265ノート

反応式

HRID 358265 の反応式
[O:1]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[O:14]C)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.I.C(OC(=O)C)(=O)C.O>CCOCC.C(O)(=O)C>[O:1]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[OH:14])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 4

HCID 962WaterHCID 7918Acetic AnhydrideHCID 24841Hydrogen iodideHCID 2487582-Methoxyphenyl phenyl ether

生成物 1

HCID 754912-Hydroxydiphenyl ether収率 83.9%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 10 g of o-phenoxyanisol, 80 ml of hydroiodic acid (52%), 80 ml of acetic acid and 40 ml of acetic anhydride was refluxed for 1.5 hours. After being cooled, the reaction mixture was poured into ice-water to deposit a precipitate. The precipitate was dissolved in ether, and the solution was washed with an aqueous saturated sodium chloride solution, an aqueous saturated thiosulfuric acid aqueous solution and then an aqueous saturated sodium chloride solution. This ether solution was dried over anhydrous sodium sulfate, and the solvent was removed to give yellow solids. The solids were dissolved in acetic acid and stirred. The mixture was poured into cold water to deposit crystals. The crystals were washed with water and then with n-hexane, and dried at 80° C. under reduced pressure to obtain 7.8 g of o-phenoxyphenol as slightly yellow powders.

後処理

  1. temperaturewas refluxed for 1.5 hours
  2. temperatureAfter being cooled
  3. washthe solution was washed with an aqueous saturated sodium chloride solution
  4. dry with materialThis ether solution was dried over anhydrous sodium sulfate
  5. customthe solvent was removed
  6. customto give yellow solids
  7. washThe crystals were washed with water
  8. dry with materialwith n-hexane, and dried at 80° C. under reduced pressure

出典と根拠

ORDレコード
ord-210b72ce6c7d44fd90a6799f26cc4adf
出典データセット
uspto-grants-1984_08
特許番号
US04465851

反応ノート

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