4,4'-Difluorobenzophenone → N-(5-uracil-yl)-4,4'-difluorobenzophenone imine

HRID 905524

Reaktionsgleichung

Reaktionsgleichung von HRID 905524
[NH2:1][C:2]1[C:3](=[O:9])[NH:4][C:5](=[O:8])[NH:6][CH:7]=1.[F:10][C:11]1[CH:25]=[CH:24][C:14]([C:15]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)=O)=[CH:13][CH:12]=1>CN1CCCC1=O.C1(N2CCCC2=O)CCCCC1>[NH:6]1[CH:7]=[C:2]([N:1]=[C:15]([C:14]2[CH:24]=[CH:25][C:11]([F:10])=[CH:12][CH:13]=2)[C:17]2[CH:18]=[CH:19][C:20]([F:23])=[CH:21][CH:22]=2)[C:3](=[O:9])[NH:4][C:5]1=[O:8]

Komponenten

4

Edukt 2

HCID 95824,4'-DifluorobenzophenoneHCID 136115-Aminouracil

Produkt 1

HCID 59595635N-(5-uracil-yl)-4,4'-difluorobenzophenone imine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 22921433N-methylpyrrolidone N-cyclohexylpyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

In a round bottom flask equipped with an overhead stirrer, 1.16 grams (0.009 mole) of 5-aminouracil was charged along with 6 grams (0.027 mole) of 4,4′-difluorobenzophenone and a N-methylpyrrolidone/N-cyclohexylpyrrolidone solvent mixture (50/50, 20 milliliters). The reaction mixture was then heated to 180° C. for 3 days. A charge of hexanes (100 milliliters) was added to fully induce precipitation, and the solid was isolated by filtration and twice recrystallized from isopropanol. The product was rinsed with isopropanol, suction dried, and vacuum dried in an oven overnight.

Aufarbeitung

  1. customIn a round bottom flask equipped with an overhead stirrer
  2. additionwas added to fully induce precipitation
  3. customthe solid was isolated by filtration
  4. customtwice recrystallized from isopropanol
  5. washThe product was rinsed with isopropanol, suction
  6. customdried
  7. customvacuum dried in an oven overnight

Quellen und Nachweise

ORD-Eintrag
ord-314ea98ef5c84e3f9777b506754f39c3
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08012541B2

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