1-Butanol → 1,1-Dibutoxycyclohexane

HRID 482143

반응식

HRID 482143 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 2437181,1-Dibutoxycyclohexane수율 182.2%

시약·촉매·용매 2

HCID 24591Bismuth trichloride촉매HCID 1140Toluene용매

반응 조건

온도
10 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-b875a7393a85409cb8f86ed45dbcfed7
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05792876

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