Potassium Carbonate → HCID 58276234, Verbindung

HRID 471826

Reaktionsgleichung

Reaktionsgleichung von HRID 471826
[Br:1][C:2]1[CH:3]=[C:4]([C:8]2[N:12]=[CH:11][NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[C:13]([O-])([O-])=O.[K+].[K+].ClC[CH2:21][C:22]([CH3:27])([CH3:26])[C:23]([O-:25])=[O:24]>CC#N>[CH3:21][C:22]([CH3:27])([CH3:26])[C:23]([O:25][CH2:13][N:10]1[CH:11]=[N:12][C:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Br:1])[CH:3]=2)=[N:9]1)=[O:24]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 124615465-(3-Bromophenyl)-1H-1,2,4-triazoleHCID 217530474-Chloro-2,2-dimethylbutanoate

Produkt 1

HCID 58276234HCID 58276234, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A slurry of 3-(3-bromophenyl)-1H-1,2,4-triazole (58.5 g; 261 mmol; Step 1 above), anhydrous K2CO3 (43.2 g; 313 mmol), and chloromethylpivalate (45 mL; 313 mmol) in dry MeCN (250 mL) was heated to 80° C. (Note 1) for 1 hour. The mixture was cooled, solid was collected by filtration and the filtrate was concentrated in vacuo. Residue from the filtaret was combined with the filtered solid and the whole was stirred with water approximately 20 minutes. Solid was collected by filtration, washed with water (×3) and recrystallized from MeOH/water, affording the title compound as a colorless solid. LC/MS (method E) tR 0.88 min, m/z 338, 340 (M+H, Br isotopes).

Aufarbeitung

  1. temperatureThe mixture was cooled
  2. filtrationsolid was collected by filtration
  3. concentrationthe filtrate was concentrated in vacuo
  4. filtrationSolid was collected by filtration
  5. washwashed with water (×3)
  6. customrecrystallized from MeOH/water

Quellen und Nachweise

ORD-Eintrag
ord-a20f4023092e43399ab9bce74f429690
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08633175B2

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