1-Butanol → 1,1-Dibutoxycyclohexane

HRID 482143

反応式

HRID 482143 の反応式
[C:1]1(=[O:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:8]([OH:12])[CH2:9][CH2:10][CH3:11].S([O-])([O-])(=O)=O.[Mg+2]>[Bi](Cl)(Cl)Cl.C1(C)C=CC=CC=1>[CH2:6]([O:7][C:1]1([O:12][CH2:8][CH2:9][CH2:10][CH3:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)[CH2:1][CH2:2][CH3:3]

参加物

6

反応物 3

HCID 2631-ButanolHCID 7967CyclohexanoneHCID 24083Sulfuric acid magnesium salt (1:1)

生成物 1

HCID 2437181,1-Dibutoxycyclohexane収率 182.2%

試薬・触媒・溶媒 2

HCID 24591Bismuth trichloride触媒HCID 1140Toluene溶媒

反応条件

温度
10 °C

実験手順

In a 300-ml three-necked flask, 98 g of cyclohexanone, 148 g of n-butanol, 50 g of anhydrous magnesium sulfate, 2 mg of bismuth chloride and 80 g of toluene were charged. The resulting mixture was stirred at 10° C. under atmospheric pressure for 10 hours in a nitrogen atmosphere. After magnesium sulfate was removed from the reaction mixture, the solvent (toluene) and unreacted starting materials were distilled off under reduced pressure. Distillation of the residue under reduced pressure gave 207.7 g of cyclohexanone dibutyl acetal (yield: 89.4%).

後処理

  1. customAfter magnesium sulfate was removed from the reaction mixture
  2. distillationwere distilled off under reduced pressure
  3. distillationDistillation of the residue under reduced pressure

出典と根拠

ORDレコード
ord-b875a7393a85409cb8f86ed45dbcfed7
出典データセット
uspto-grants-1998_08
特許番号
US05792876

関連ノート

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