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Ammonia → HCID 25184712, Verbindung

HRID 1878066
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1878066
[Cl:1][CH2:2][C:3]([NH:5][C:6]1[CH:7]=[N:8][C:9]([C:12](=[N:14][OH:15])[NH2:13])=[CH:10][CH:11]=1)=[O:4].N.[C:17](OC(=O)C)(=O)[CH3:18]>O>[Cl:1][CH2:2][C:3]([NH:5][C:6]1[CH:7]=[N:8][C:9]([C:12]2[N:13]=[C:17]([CH3:18])[O:15][N:14]=2)=[CH:10][CH:11]=1)=[O:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 222AmmoniaHCID 7918Acetic AnhydrideHCID 137068883HCID 137068883, Verbindung

Produkt 1

HCID 25184712HCID 25184712, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Compound of example 4 (5.5 g, 24 mmol) was refluxed in acetic anhydride (10 mL) at a temperature in the range of 115-120° C. for 2 hours. The black colored reaction mixture was cooled, diluted with water, basified with ammonia solution, and extracted with ethyl acetate (3×100 mL). The organic layer was washed with brine, dried over sodium sulfate and concentrated. The crude product obtained was purified over silica gel using ethyl acetate/petroleum ether (25%-50%) as eluent and the semipurified fractions were further purified using methanol/chloroform (0.5% -1%) as eluent. Pure fractions were concentrated and crystallized using chloroform/petroleum ether, to obtain the title compound.

Aufarbeitung

  1. temperatureThe black colored reaction mixture was cooled
  2. extractionextracted with ethyl acetate (3×100 mL)
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe crude product obtained
  7. customwas purified over silica gel
  8. customthe semipurified fractions were further purified
  9. concentrationPure fractions were concentrated
  10. customcrystallized

Quellen und Nachweise

ORD-Eintrag
ord-724c10d5fe54499e984e8ef8c4090265
Quelldatensatz
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08314103B2

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