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creatinine → HCID 136074472, Verbindung

HRID 904172
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 904172
[CH3:1][N:2]1[C:7]([NH2:8])=[N:6][C:4](=[O:5])[CH2:3]1.[O:9]1[CH:13]=[CH:12][C:11]([N:14]=[C:15]=[O:16])=[CH:10]1>CN(C=O)C.C1(C)C=CC=CC=1>[O:9]1[CH:13]=[CH:12][C:11]([NH:14][C:15]([N:8]=[C:7]2[NH:6][C:4](=[O:5])[CH2:3][N:2]2[CH3:1])=[O:16])=[CH:10]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 588creatinineHCID 115283353-Isocyanatofuran

Produkt 1

HCID 136074472HCID 136074472, VerbindungAusbeute 1,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a stirred mixture of 18.3 g (162 mM) of creatinine in 120 ml of anhydrous DMF was added a solution of 17.2 g (162 mM) of 3-furanyl isocyanate in 80 ml of toluene. After stirring the mixture for 3 hrs. at 65° C., the mixture was partially concentrated under vacuum and the residue poured into 1200 ml of water. The resulting precipitate was collected, washed with water and recrystallized from ethyl acetate. The solid was then chromatographed over silica gel using ethyl acetate as the eluant and the fractions containing the product were concentrated and the residue recrystallized from toluene to give 0.5 g of the above urea as a tan solid, m.p. 179°-181° C. (dec.).

Aufarbeitung

  1. concentrationat 65° C., the mixture was partially concentrated under vacuum
  2. additionthe residue poured into 1200 ml of water
  3. customThe resulting precipitate was collected
  4. washwashed with water
  5. customrecrystallized from ethyl acetate
  6. customThe solid was then chromatographed over silica gel
  7. additionthe fractions containing the product
  8. concentrationwere concentrated
  9. customthe residue recrystallized from toluene

Quellen und Nachweise

ORD-Eintrag
ord-32fcc878990c42e8b5fbc377663e90f6
Quelldatensatz
uspto-grants-1980_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04230713

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