Isopropanol → 2-Cyclohexen-1-one, 2,5,6-trimethyl-

HRID 65802

反応式

HRID 65802 の反応式
O[CH:2]([CH3:6])[CH2:3][CH:4]=[O:5].[CH2:7]([C:9]([CH2:11]C)=O)[CH3:8].[CH:13](O)(C)C.[OH-].[Na+]>C(O)(=O)C>[CH3:13][C:3]1[C:4](=[O:5])[CH:7]([CH3:8])[CH:9]([CH3:11])[CH2:6][CH:2]=1

参加物

6

反応物 4

HCID 3776IsopropanolHCID 7288Ethyl ketone2 回HCID 78973-HydroxybutanalHCID 14798Sodium Hydroxide

生成物 1

HCID 892642-Cyclohexen-1-one, 2,5,6-trimethyl-収率 47.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 88 g of β-hydroxybutyraldehyde and 150 g of diethyl ketone is added dropwise in the course of one hour to a mixture of 250 g of diethyl ketone, 80 g of isopropanol and 5 g of sodium hydroxide powder which is boiling under reflux. The whole is boiled for another hour under reflux. Neutralization is effected with glacial acetic acid and the aqueous phase is separated. The organic layer is fractionated. 65 g of 2,5,6-trimethyl-2-cyclohexen-1-one having a boiling point of 74° to 76° C. at 12 mm Hg is obtained. The yield is 47% with reference to β-hydroxybutyraldehyde.

後処理

  1. temperatureunder reflux
  2. waitThe whole is boiled for another hour
  3. temperatureunder reflux
  4. customthe aqueous phase is separated

出典と根拠

ORDレコード
ord-c16defd56be34a8fba979fa521f18f93
出典データセット
uspto-grants-1978_12
特許番号
US04128728

関連ノート

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