Potassium Fluoride → HCID 178437211, Verbindung

HRID 45871

Reaktionsgleichung

Reaktionsgleichung von HRID 45871
[N+:1]([C:4]1[CH:5]=[C:6]([C:10]2[C:14]([C:15]#[C:16][Si](C)(C)C)=[CH:13][NH:12][N:11]=2)[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[F-].[K+]>CO>[C:15]([C:14]1[C:10]([C:6]2[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)=[N:11][NH:12][CH:13]=1)#[CH:16]

Komponenten

4

Edukt 2

HCID 522689Potassium FluorideHCID 1785041883-(3-nitrophenyl)-4-[(trimethylsilyl)ethynyl]-1H-pyrazole

Produkt 1

HCID 178437211HCID 178437211, VerbindungAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

300 mg (1.05 mmol) of 3-(3-nitrophenyl)-4-[(trimethylsilyl)ethynyl]-1H-pyrazole were suspended in 60 ml of methanol and 120 mg (2.1 mmol) of potassium fluoride were added and the mixture stirred at room temperature overnight. After this time the solvent was removed under reduced pressure and the residue taken up with dichloromethane and washed with water. The organic layer was then dried over sodium sulphate and evaporated. The crude was finally purified by flash-chromatography on a silica gel column (CH2C12-CH3COCH3 9/1), giving 150 mg (67%) of the title compound.

Aufarbeitung

  1. customAfter this time the solvent was removed under reduced pressure
  2. washwashed with water
  3. dry with materialThe organic layer was then dried over sodium sulphate
  4. customevaporated
  5. customThe crude was finally purified by flash-chromatography on a silica gel column (CH2C12-CH3COCH3 9/1)

Quellen und Nachweise

ORD-Eintrag
ord-c07ad4186b054ea08a4e12d01fe6befb
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08541575B2

Verknüpfte Notizen

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