1-Butanol → 1,1-Dibutoxycyclohexane

HRID 482138

반응식

HRID 482138 반응식
O.[C:2]1(=[O:8])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[CH2:9]([OH:13])[CH2:10][CH2:11][CH3:12]>C1(C)C=CC=CC=1>[CH2:7]([O:8][C:2]1([O:13][CH2:9][CH2:10][CH2:11][CH3:12])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1)[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 3

HCID 2631-ButanolHCID 962WaterHCID 7967Cyclohexanone

생성물 1

HCID 2437181,1-Dibutoxycyclohexane수율 187.7%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
125 °C

실험 절차

In a 300-ml three-necked flask equipped with a water separator, 98 g (1 mole) of cyclohexanone, 148 g (2 moles) of n-butanol, 2.4 mg of stannous chloride dihydrate and 40 g of toluene were charged. The resulting mixture was heated at 125° C. under atmospheric pressure for 6 hours in a nitrogen atmosphere while removing the water formed from the reaction mixture by azeotropic distillation. When water was no longer distilled, the solvent (toluene) and unreacted starting materials were distilled off under reduced pressure. Distillation of the residue under reduced pressure gave 214.3 g of cyclohexanone dibutyl acetal [R1, R2 =a pentamethylene group and R3 =a n-butyl group] (boiling point: 102° C./3 mmHg) (yield: 94.0%).

후처리

  1. additionwere charged
  2. customwhile removing the water
  3. customformed from the reaction mixture by azeotropic distillation
  4. distillationWhen water was no longer distilled
  5. distillationwere distilled off under reduced pressure
  6. distillationDistillation of the residue under reduced pressure

출처 및 근거

ORD 기록
ord-542f35a4804e41f38e9363201eecef33
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05792876

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