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Diethyl Ether → Ethyl 4-(4-chlorophenyl)-4-oxobut-2-enoate

HRID 1981872
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반응식

HRID 1981872 반응식
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([CH:8]=[CH:9][C:10]([OH:12])=[O:11])=[O:7])=[CH:4][CH:3]=1.S(OC)(OC)(=O)=O.C(=O)([O-])[O-].[K+].[K+].[CH2:28](OCC)[CH3:29]>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([CH:8]=[CH:9][C:10]([O:12][CH2:28][CH3:29])=[O:11])=[O:7])=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 346433-(4-Chlorobenzoyl)-acrylic acid

생성물 1

HCID 54524585Ethyl 4-(4-chlorophenyl)-4-oxobut-2-enoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4.22 g of 3-(4-chlorobenzoyl)-acrylic acid in 40 ml of dimethylformamide were added 3.68 g of dimethyl sulfate and 1.36 g of potassium carbonate, and the mixture was stirred at room temperature for 3 hours. To the reaction solution was added diethyl ether. The mixture was washed, in turn, with water, a saturated aqueous solution of sodium hydrogencarbonate and water, and dried over magnesium sulfate. The diethyl ether was removed from the mixture by evaporation, and the residue was recrystallized from hexane to give 2.68 g of ethyl 3-(4-chlorobenzoyl)acrylate.

후처리

  1. washThe mixture was washed, in turn, with water
  2. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and water, and dried over magnesium sulfate
  3. customThe diethyl ether was removed from the mixture by evaporation
  4. customthe residue was recrystallized from hexane

출처 및 근거

ORD 기록
ord-723585dfc30a441eaedcd54918fb7303
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04594197

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