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Methyl iodide → HCID 68418565, Verbindung

HRID 2366539
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2366539
[H-].[Na+].[O:3]=[C:4]1[NH:8][CH2:7][CH2:6][N:5]1[CH:9]1[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:16])[CH2:11][CH2:10]1.[CH3:25]I>CN(C=O)C>[CH3:25][N:8]1[CH2:7][CH2:6][N:5]([CH:9]2[CH2:10][CH2:11][N:12]([C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:16])[CH2:13][CH2:14]2)[C:4]1=[O:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 23463818Benzyl 4-(2-oxoimidazolidin-1-yl)piperidine-1-carboxylate

Produkt 1

HCID 68418565HCID 68418565, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Sodium hydride (80 mg) was added to a solution of benzyl 4-(2-oxoimidazolidin-1-yl)piperidin-1-carboxylate (0.30 g) in DMF (5 mL), the mixture was stirred at room temperature for 30 minutes. After addition of methyl iodide (0.25 mL), the mixture was stirred at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, diluted with water, and extracted with ethyl acetate. The extract was washed with water, an aqueous 5% citric acid solution and saturated saline solution and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to obtain the title compound (0.32 g, quantitative) as a colorless oil.

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature for 15 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additiondiluted with water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialan aqueous 5% citric acid solution and saturated saline solution and dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-01f1bac7dd84405c8b5bdbc360125a3e
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08697865B2

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