Hydrochloric Acid → HCID 178437869, Verbindung

HRID 2257040Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2257040
[Na].[CH:2]1([N:7]2[C:11]([NH2:12])=[C:10]([C:13]([NH2:15])=[O:14])[C:9]([CH2:16][CH3:17])=[N:8]2)[CH2:6][CH2:5][CH2:4][CH2:3]1.[F:18][C:19]([F:33])([F:32])[C:20]1[CH:25]=[CH:24][C:23]([CH2:26][C:27](OCC)=O)=[CH:22][CH:21]=1.Cl>C(O)C.O>[CH:2]1([N:7]2[C:11]3=[N:12][C:27]([CH2:26][C:23]4[CH:22]=[CH:21][C:20]([C:19]([F:18])([F:32])[F:33])=[CH:25][CH:24]=4)=[N:15][C:13](=[O:14])[C:10]3=[C:9]([CH2:16][CH3:17])[NH:8]2)[CH2:3][CH2:4][CH2:5][CH2:6]1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 5360545SodiumHCID 14134124Ethyl (4-(trifluoromethyl)phenyl)acetateHCID 224493525-amino-1-cyclopentyl-3-ethyl-1H-pyrazole-4-carboxamide

Produkt 1

HCID 178437869HCID 178437869, VerbindungAusbeute 57,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Sodium (622 mg) was dissolved in ethanol (45 mL) and then 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (3.0 g, 13.5 mmol), followed by ethyl 4-trifluoromethylphenylacetate (6.27 g, 27 mmol) were added. The reaction mixture was refluxed overnight, cooled to room temperature, and the solvent was stripped. Water, followed by 2N HCl were added to the residue and the product was collected by filtration, recrystallized from ether and dried at 110° C. and 0.2 mm Hg to afford 3.03 g of 1-cyclopentyl-3-ethyl-6-(4-trifluoromethylphenylmethyl) pyrazolo[3,4-d]pyrimidin-4-one, m.p. 212°-213° C.

Aufarbeitung

  1. additionwere added
  2. temperatureThe reaction mixture was refluxed overnight
  3. additionwere added to the residue
  4. filtrationthe product was collected by filtration
  5. customrecrystallized from ether
  6. customdried at 110° C.

Quellen und Nachweise

ORD-Eintrag
ord-2e5d1827b3b04be6a1942a140e73c1ae
Quelldatensatz
uspto-grants-1997_08
Patentnummer
US05656629

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