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2,5,8,11,14,17,20-Heptaoxadocosan-22-amine → HCID 178496251, Verbindung

HRID 1527633
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1527633
[N:1]1([C:6]([NH:8][C:9]2[NH:10][C:11]([CH3:16])=[CH:12][C:13](=[O:15])[N:14]=2)=[O:7])[CH:5]=[CH:4]N=C1.C[O:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][O:30][CH2:31][CH2:32][O:33][CH2:34][CH2:35][O:36][CH2:37]CN>C(OCC)(=O)C>[CH3:37][O:36][CH2:35][CH2:34][O:33][CH2:32][CH2:31][O:30][CH2:29][CH2:28][O:27][CH2:26][CH2:25][O:24][CH2:23][CH2:22][O:21][CH2:20][CH2:19][O:18][CH2:4][CH2:5][NH:1][C:6]([NH:8][C:9]1[NH:10][C:11]([CH3:16])=[CH:12][C:13](=[O:15])[N:14]=1)=[O:7]
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Komponenten

4

Edukt 2

HCID 187646512,5,8,11,14,17,20-Heptaoxadocosan-22-amineHCID 178429402HCID 178429402, Verbindung

Produkt 1

HCID 178496251HCID 178496251, VerbindungAusbeute 60,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a suspension of 4.38 g of 2-(1-imidazolylcarbonylamino)-6-methyl-4[1H]-pyrimidinone 1A (0.02 mol) in 200 ml of ethyl acetate were added 7.4 g of 2,5,8,11,14,17,20 heptaoxadocosan-22-amine (0.0218 mol). The reaction mixture was refluxed for 12 hours. The mixture was then allowed to return to room temperature, and was evaporated under reduced pressure. The residue was taken up in acetone (50 ml) and then filtered to remove the imidazole. The filtrate was evaporated under reduced pressure and then taken up again in 50 ml of acetone and filtered. The filtrate was evaporated under reduced pressure. 5.9 g of the expected product were thus obtained in the form of a pasty oil, in a yield of 60%. 1H and 13C NMR spectra compliant.

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 12 hours
  2. customto return to room temperature
  3. customwas evaporated under reduced pressure
  4. filtrationfiltered
  5. customto remove the imidazole
  6. customThe filtrate was evaporated under reduced pressure
  7. filtrationfiltered
  8. customThe filtrate was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c0c3b82db4ff4723bc9c7ea117dc9942
Quelldatensatz
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09089500B2

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