Sodium → HCID 23020439, Verbindung

HRID 747166Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 747166
[Na].F[C:3]1[CH:8]=[C:7]([C:9]2[C:10]([C:21]3[O:22][CH:23]=[CH:24][CH:25]=3)=[N:11][C:12]([NH2:20])=[N:13][C:14]=2[C:15]2[O:16][CH:17]=[CH:18][CH:19]=2)[CH:6]=[CH:5][N:4]=1>C(O)CCC>[CH2:15]([O:16][C:3]1[CH:8]=[C:7]([C:9]2[C:10]([C:21]3[O:22][CH:23]=[CH:24][CH:25]=3)=[N:11][C:12]([NH2:20])=[N:13][C:14]=2[C:15]2[O:16][CH:17]=[CH:18][CH:19]=2)[CH:6]=[CH:5][N:4]=1)[CH2:14][CH2:9][CH3:7]

Komponenten

4

Edukt 2

HCID 5360545SodiumHCID 23020419HCID 23020419, Verbindung

Produkt 1

HCID 23020439HCID 23020439, VerbindungAusbeute 108 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

In a reaction vessel, sodium (21 mg, 0.931 mmol) was dissolved in n-butanol (4 ml) and then 5-(2-fluoro-4-pyridyl)-4,6-di(2-furyl)-2-pyrimidinamine (100 mg, 0.310 mmol) was added thereto, followed by stirring under reflux for 5 hours under an atmosphere of nitrogen gas. The reaction was terminated by adding water thereto. Then, the reaction mixture was extracted with ethyl acetate, washed with water and brine, dried over anhydrous sodium sulfate and then the filtrate was concentrated. The resulting solid was suspended in ethanol, collected by filtration and washed with ethanol, to give the title compound (63 mg, 54%) as a pale yellow solid.

Aufarbeitung

  1. temperatureunder reflux for 5 hours under an atmosphere of nitrogen gas
  2. customThe reaction was terminated
  3. additionby adding water
  4. extractionThen, the reaction mixture was extracted with ethyl acetate
  5. washwashed with water and brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationthe filtrate was concentrated
  8. filtrationcollected by filtration
  9. washwashed with ethanol

Quellen und Nachweise

ORD-Eintrag
ord-e04d12db90154c5a916a472b01277a57
Quelldatensatz
uspto-grants-2008_07
Patentnummer
US07396836B2

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