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Sodium Chloride → N-[5-(3,4-dihydroxyphenyl)-2,4-pentadienoyl]--N'-(2-benzhydroxyethyl)piperazine

HRID 652969
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 652969
[CH:1]([O:14][CH2:15][CH2:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.COCCOC[O:29][C:30]1[CH:31]=[C:32]([CH:43]=[CH:44][CH:45]=[CH:46][C:47](N2CCSC2=S)=[O:48])[CH:33]=[CH:34][C:35]=1[O:36]COCCOC.C(Cl)(Cl)Cl.CO.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[Cl-].[Na+].C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O.COCCOCOC1C=C(C=CC=CC(N2CCN(CCOC(C3C=CC=CC=3)C3C=CC=CC=3)CC2)=O)C=CC=1OCOCCOC.CO>[OH:29][C:30]1[CH:31]=[C:32]([CH:43]=[CH:44][CH:45]=[CH:46][C:47]([N:20]2[CH2:19][CH2:18][N:17]([CH2:16][CH2:15][O:14][CH:1]([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH2:22][CH2:21]2)=[O:48])[CH:33]=[CH:34][C:35]=1[OH:36]
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Komponenten

10

Edukt 6

HCID 5234Sodium ChlorideHCID 10340Sodium CarbonateHCID 521998p-Toluenesulfonic acid monohydrateHCID 6485251-[2-(Diphenylmethoxy)ethyl]piperazineHCID 21584188Chloroform methanolHCID 54009022N-[5-[3,4-di(beta-methoxyethoxymethoxy)phenyl]2,4-pentadienoyl]thiazolidine-2-thione

Produkt 1

HCID 54013656N-[5-(3,4-dihydroxyphenyl)-2,4-pentadienoyl]--N'-(2-benzhydroxyethyl)piperazineAusbeute 38,9 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 54258742N-[5-[3,4-bis(beta-methoxyethoxymethoxy)phenyl]-2,4-pentadienoyl]-N'-(2-benzhydroxyethyl)piperazineLösungsmittel

Versuchsvorschrift

To a solution of 690 mg (2.33 mmol) of N-(2- benzhydroxyethyl)piperazine in dry dimethylformamide (2 ml) was added 1.75 g (3.26 mmol) of N-[5-[3,4-bis(βmethoxyethoxymethoxy)phenyl]-2,4-pentadienoyl]thiazolidine-2-thione, and the mixture was reacted at room temperature 18 hours under argon atmosphere. The reaction mixture was concentrated by evaporation under reduced pressure and the residue was subjected to silica gel column chromatography. There was obtained from fractions eluted with chloroform - methanol (100:1) 856 mg (1.30 mmol) of N-[5-[3,4-bis(β-methoxyethoxymethoxy)phenyl]-2,4-pentadienoyl]-N'-(2-benzhydroxyethyl)piperazine. To a solution of 856 mg (1.30 mmol) of the amide compound in methanol (17 ml) was added 257 mg (1.35 mmol) of p-toluenesulfonic acid monohydrate, and the mixture was refluxed for 4 hours. A saturated aqueous solution of sodium chloride was added to the reaction mixture, which was adjusted to a pH value of 10 by the addition of an aqueous solution of sodium carbonate, and then extracted with ethyl acetate. The organic layer was washed with water and concentrated by evaporation under reduced pressure. The residue was subjected to Sephadex column chromatography, eluted with methanol, to give 439 mg (0.906 mmol) of N-[5-(3,4-dihydroxyphenyl)-2,4-pentadienoyl]--N'-(2-benzhydroxyethyl)piperazine. Spectrophotometric data of the product support the structure shown below. ##STR97##

Aufarbeitung

  1. customthe mixture was reacted at room temperature 18 hours under argon atmosphere
  2. concentrationThe reaction mixture was concentrated by evaporation under reduced pressure
  3. customThere was obtained from fractions
  4. temperaturethe mixture was refluxed for 4 hours
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. concentrationconcentrated by evaporation under reduced pressure
  8. washeluted with methanol

Quellen und Nachweise

ORD-Eintrag
ord-0950a9bd1b21402087974c10855da3a5
Quelldatensatz
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04673684

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