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Potassium Iodide → HCID 19874550, Verbindung

HRID 465455
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 465455
[CH2:1]([C:5]1[CH:22]=[CH:21][C:8]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]Br)=[CH:7][CH:6]=1)[C:2]([CH3:4])=[O:3].C(=O)([O-])[O-].[K+].[K+].Cl.[NH:30]1[CH2:34][CH2:33][C:32](=[O:35])[NH:31]1.[I-].[K+]>C(#N)C.O>[CH2:1]([C:5]1[CH:22]=[CH:21][C:8]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][N:30]2[CH2:34][CH2:33][C:32](=[O:35])[NH:31]2)=[CH:7][CH:6]=1)[C:2]([CH3:4])=[O:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 2733712Pyrazolidin-3-one hydrochlorideHCID 19874510HCID 19874510, Verbindung

Produkt 1

HCID 19874550HCID 19874550, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 18373917
Acetonitrile--water (1/1)
Lösungsmittel

Versuchsvorschrift

A mixture of 10-(4-acetonylphenoxy)decylbromide, ethylene ketal (3.0 g), potassium carbonate (3.8 g), pyrazolidin-3-one hydrochloride (1.47 g) and potassium iodide (0.5 g) in acetonitrile:water (95:5), was heated under reflux for 3 hr. The reaction mixture was allowed to cool, filtered and the solvent evaporated in vacuo. The residue was dissolved in chloroform, washed with water (2×50 ml), dried (magnesium sulphate), fitered and the solvent removed in vacuo. The residue was dissolved in acetone (50 ml) and treated with 2M hydrochloric acid solution (3 ml) and allowed to stand at room temperature for 3 hr. The solvent was removed in vacuo and the residue was dissolved in chloroform and washed with 1.2M sodium bicarbonate solution (1×50 ml), water (2×50 ml), dried (magnesium sulphate), filtered and the solvent removed in vacuo to give 1-[10-(4-acetonylphenoxy)decyl]pyrazolidin-3-one (0.66 g).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hr
  3. temperatureto cool
  4. filtrationfiltered
  5. customthe solvent evaporated in vacuo
  6. dissolutionThe residue was dissolved in chloroform
  7. washwashed with water (2×50 ml)
  8. dry with materialdried (magnesium sulphate)
  9. customthe solvent removed in vacuo
  10. dissolutionThe residue was dissolved in acetone (50 ml)
  11. additiontreated with 2M hydrochloric acid solution (3 ml)
  12. customThe solvent was removed in vacuo
  13. dissolutionthe residue was dissolved in chloroform
  14. washwashed with 1.2M sodium bicarbonate solution (1×50 ml), water (2×50 ml)
  15. dry with materialdried (magnesium sulphate)
  16. filtrationfiltered
  17. customthe solvent removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bcf9f90175924dc1bdf3931b33b96a7d
Quelldatensatz
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05153210

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