1-Butanol → 1,1-Dibutoxycyclohexane

HRID 482138

反応式

HRID 482138 の反応式
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]

参加物

5

反応物 3

HCID 2631-ButanolHCID 962WaterHCID 7967Cyclohexanone

生成物 1

HCID 2437181,1-Dibutoxycyclohexane収率 187.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
125 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-542f35a4804e41f38e9363201eecef33
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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