Benzene → 3,5-Dimethylcyclohexanone

HRID 1461951

反応式

HRID 1461951 の反応式
[CH3:1][CH:2]1[CH2:7][CH:6]([CH3:8])[CH2:5][CH:4]([OH:9])[CH2:3]1.C1C=CC=CC=1.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].S(=O)(=O)(O)O>C(O)(=O)C.O>[CH3:1][CH:2]1[CH2:7][CH:6]([CH3:8])[CH2:5][C:4](=[O:9])[CH2:3]1

参加物

7

反応物 4

HCID 241BenzeneHCID 1118Sulfuric AcidHCID 215843,5-Dimethylcyclohexan-1-olHCID 25408Sodium Dichromate

生成物 1

HCID 1375443,5-Dimethylcyclohexanone収率 82%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

128 g of 3,5-dimethyl-cyclohexanol and 500 ml of benzene are added to a round flask which is fitted with a stirrer, thermometer, dropping funnel and reflux condenser. While stirring and cooling there is now slowly added dropwise thereto a mixture of 119 g of sodium dichromate, 500 ml of water, 162 ml of concentrated sulphuric acid and 50 ml of glacial acetic acid. Thereby the temperature should not exceed +10° C. The mixture is stirred at this temperature for a further 3 hours and then the organic phase is separated. The aqueous phase is diluted with 130 ml of water and extracted with benzene. The combined organic phases are washed neutral and concentrated. The residue is distilled over a Widmer column and gives 102.7 g of 3,5-dimethyl-cyclohexanone.

後処理

  1. customis fitted with a stirrer
  2. temperaturereflux condenser
  3. temperaturecooling there
  4. additionis now slowly added dropwise
  5. customexceed +10° C
  6. stirringThe mixture is stirred at this temperature for a further 3 hours
  7. customthe organic phase is separated
  8. additionThe aqueous phase is diluted with 130 ml of water
  9. extractionextracted with benzene
  10. washThe combined organic phases are washed neutral
  11. concentrationconcentrated
  12. distillationThe residue is distilled over a Widmer column

出典と根拠

ORDレコード
ord-23136cae7554498d89ff9583634aa141
出典データセット
uspto-grants-1984_07
特許番号
US04457862

関連ノート

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