Hydrogen Bromide → 4,4'-(Cycloheptane-1,1-diyl)diphenol

HRID 27800

反応式

HRID 27800 の反応式
[C:1]1(=O)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:9]1([OH:15])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.Br>>[C:1]1([C:12]2[CH:13]=[CH:14][C:9]([OH:15])=[CH:10][CH:11]=2)([C:12]2[CH:13]=[CH:14][C:9]([OH:15])=[CH:10][CH:11]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 3

HCID 260Hydrogen Bromide2 回HCID 996PhenolHCID 10400Cycloheptanone

生成物 1

HCID 134848914,4'-(Cycloheptane-1,1-diyl)diphenol

実験手順

Into a solution of 112.7 parts by weight (1.0 partmole) cycloheptanone and 470 parts by weight (5.0 partmole) phenol there was introduced gaseous hydrobromic acid. The mildly exothermic reaction was moderated by external cooling, keeping the reaction temperature between 30° and 37° C. after ca. 1.5 hour of reaction time, the red colored mixture thickened and solids began to form. After an additional four hour contact with a slow stream of hydrobromic acid, all acid was removed by placing the stirred mixture under water aspirator vacuum and the solid phase removed by vacuum filtration. Washing the solids with hot water and recrystallizing them by charcoaling from aqueous menthol, yielded white crystals of 4,4'-cycloheptylidenediphenol, melting point 208°-209° C., that were 99.1% pure by gas chromatography analysis (retention time: 25.35 min.; p-cumylphenol reference retention time: 16.47 min.).

後処理

  1. customThe mildly exothermic reaction
  2. customthe reaction temperature between 30° and 37° C.
  3. customafter ca. 1.5 hour
  4. customof reaction time
  5. customto form
  6. customall acid was removed
  7. customthe solid phase removed by vacuum filtration
  8. washWashing the solids with hot water
  9. customrecrystallizing them

出典と根拠

ORDレコード
ord-a0e6aa494f5f44228088d1199964be84
出典データセット
uspto-grants-1980_09
特許番号
US04223170

関連ノート

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