Cycloheptylbenzene → 4-Cycloheptyl-benzaldehyde

HRID 1415326

반응식

HRID 1415326 반응식
[CH:1]1([C:8]2[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=2C=O)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1(C2C=CC=CC=2)CCCCCC1.Cl[CH:30]([O:32]C(Cl)Cl)Cl>C(Cl)Cl.[Ti](Cl)(Cl)(Cl)Cl>[CH:1]1([C:8]2[CH:9]=[CH:12][C:13]([CH:30]=[O:32])=[CH:14][CH:15]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]1

참가 물질

6

반응물 3

HCID 297933CycloheptylbenzeneHCID 558102Bis(dichloromethyl) etherHCID 21484447Cycloheptylbenzaldehyde

생성물 1

HCID 214844454-Cycloheptyl-benzaldehyde

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매

반응 조건

온도
10 °C

실험 절차

Cycloheptylbenzaldehyde can be manufactured as follows: 200 ml of titanium tetrachloride are added dropwise, whilst stirring, to a solution of 200 g of cycloheptylbenzene in 600 ml of absolute methylene chloride under a nitrogen atmosphere at -10° C, and thereafter 132.5 g of dichloromethyl ether are added similarly at 0° C. The reaction mixture is then stirred for a further 30 minutes at 10° C and poured onto 3 kg of ice, and the whole is extracted twice with 500 ml of methylene chloride. The organic phases are washed with water, dried over sodium sulphate and evaporated to dryness in vacuo. Distillation of the evaporation residue in a high vacuum yields 4-cycloheptyl-benzaldehyde in the fraction boiling at 120°-130° C/0.8 mm Hg.

후처리

  1. extractionthe whole is extracted twice with 500 ml of methylene chloride
  2. washThe organic phases are washed with water
  3. dry with materialdried over sodium sulphate
  4. customevaporated to dryness in vacuo
  5. distillationDistillation of the evaporation residue in a high vacuum

출처 및 근거

ORD 기록
ord-f0dd31afe171456187fe90f4a2bda7de
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04004026

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