Acetone → Ethyl 4-(2,4-nonadiynyloxy)-benzoate

HRID 2639

반응식

HRID 2639 반응식
[OH:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:19][C:20]([CH3:22])=O>CCCCCC.C(OCC)(=O)C>[CH2:19]([O:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:11][CH:12]=1)[C:20]#[C:22][C:12]#[C:2][CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

5

반응물 3

HCID 180AcetoneHCID 8434EthylparabenHCID 11430Potassium Carbonate

생성물 1

HCID 18935880Ethyl 4-(2,4-nonadiynyloxy)-benzoate수율 70%

시약·촉매·용매 1

HCID 21226206Ethyl acetate hexane용매

실험 절차

In a flask were placed 3.78 g (0.024 mole) of 1-chloro-2,4-nonadiyne thus obtained, 3.32 g (0.02 mole) of ethyl 4-hydroxybenzoate, 5.5 g (0.04 mole) of potassium carbonate, and 50 ml of acetone and the mixture was refluxed by heating for 11 hours. After allowing to cool the reaction mixture to room temperature, the reaction mixture was poured in 250 ml of ice-water and the product was extracted with methylene chloride. After distilling off the solvent of the organic layer, the residue formed was purified by a silica gel column chromatography(developing solvent: hexane/ethyl acetate=3/1) to provide 4.0 g (yield 70%) of ethyl 4-(2,4-nonadiynyloxy)-benzoate.

후처리

  1. temperatureby heating for 11 hours
  2. extractionthe product was extracted with methylene chloride
  3. distillationAfter distilling off the solvent of the organic layer
  4. customthe residue formed
  5. customwas purified by a silica gel column chromatography(developing solvent

출처 및 근거

ORD 기록
ord-e5b29654fa7b4c0a9addc6161d045c21
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05730903

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