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Water → 4-Oxocyclohexane-1-carbaldehyde

HRID 653361
ノート
印刷プレビュー

反応式

HRID 653361 の反応式
C1CO[C:3]2([CH2:8][CH2:7][C:6](=[CH:9][O:10]C)[CH2:5][CH2:4]2)[O:2]1.O>C(O)(=O)C>[CH:9]([CH:6]1[CH2:7][CH2:8][C:3](=[O:2])[CH2:4][CH2:5]1)=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 962WaterHCID 552771378-(Methoxymethylene)-1,4-dioxaspiro[4.5]decane

生成物 1

HCID 111709734-Oxocyclohexane-1-carbaldehyde収率 93%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 10.55 g of 1,1-ethylenedioxy-4-(methoxymethylene)cyclohexane, 130 ml of water and 200 ml of glacial acetic acid was heated to reflux for 1 hour. The solvent was subsequently distilled off on a rotary evaporator and the distillate was extracted twice with methylene chloride. The distillation residue (a yellow oil) was diluted with 200 ml of water, neutralized with sodium carbonate solution and extracted three times with methylene chloride. The organic phases were washed with saturated sodium carbonate solution and the aqueous phases were back-extracted with methylene chloride. The organic phases were dried over magnesium sulphate and evaporated. Distillation of the residual, yellow oil gave 6.7 g (93%) of 4-formylcyclohexanone at 70° C./0.15 Torr.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 1 hour
  3. distillationThe solvent was subsequently distilled off on a rotary evaporator
  4. extractionthe distillate was extracted twice with methylene chloride
  5. additionThe distillation residue (a yellow oil) was diluted with 200 ml of water
  6. extractionextracted three times with methylene chloride
  7. washThe organic phases were washed with saturated sodium carbonate solution
  8. extractionthe aqueous phases were back-extracted with methylene chloride
  9. dry with materialThe organic phases were dried over magnesium sulphate
  10. customevaporated
  11. distillationDistillation of the residual, yellow oil

出典と根拠

ORDレコード
ord-3feb445cc3524f229a6ab9d1b45098f3
出典データセット
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04676604

反応ノート

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