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Butanal → n-Butanal dicrotyl acetal

HRID 482144
노트
인쇄 미리보기

반응식

HRID 482144 반응식
[CH:1](=[O:5])[CH2:2][CH2:3][CH3:4].[CH2:6]([OH:10])[CH:7]=[CH:8][CH3:9]>C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.[Ti].C1(C)C=CC=CC=1>[CH2:1]([O:5][CH:6]([O:10][CH2:1][CH:2]=[CH:3][CH3:4])[CH2:7][CH2:8][CH3:9])[CH:2]=[CH:3][CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 261ButanalHCID 200242-Buten-1-ol

생성물 1

HCID 57271298n-Butanal dicrotyl acetal수율 190.7%

시약·촉매·용매 2

HCID 44629996tetrakis((Z)-4-hydroxypent-3-en-2-one);titanium촉매HCID 1140Toluene용매

반응 조건

온도
20 °C

실험 절차

In a 300-ml three-necked flask, 72 g (1 mole) of n-butanal, 144 g of crotyl alcohol, 3 mg of titanium acetylacetonate, 80 g of molecular sieve 4A and 50 g of toluene were charged. The resulting mixture was stirred at 20° C. under atmospheric pressure for 12 hours in a nitrogen atmosphere. After the removal of the molecular sieve 4A from the reaction mixture, the solvent (toluene) and the unreacted starting materials were distilled off under reduced pressure. Distillation of the residue under reduced pressure gave 189.1 g of n-butanal dicrotyl acetal (boiling point: 116° C./25 mmHg) (yield: 95.5%).

후처리

  1. customAfter the removal of the molecular sieve 4A from the reaction mixture
  2. distillationthe solvent (toluene) and the unreacted starting materials were distilled off under reduced pressure
  3. distillationDistillation of the residue under reduced pressure

출처 및 근거

ORD 기록
ord-1083e6383f0346da8a1eb6f0d2893a8a
출처 데이터셋
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05792876

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