Dimethylformamide dimethyl acetal → HCID 178484244, Verbindung

HRID 452972

Reaktionsgleichung

Reaktionsgleichung von HRID 452972
[C:1]([C:5]1[CH:9]=[C:8]([NH2:10])[NH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].CO[CH:13](OC)[N:14]([CH3:16])[CH3:15]>>[C:1]([C:5]1[CH:9]=[C:8](/[N:10]=[CH:13]/[N:14]([CH3:16])[CH3:15])[NH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2]

Komponenten

3

Versuchsvorschrift

A mixture of 3-tert-butyl-1H-pyrazol-5-amine (5 g, 36 mmol, Alfa-aesar) and N,N-dimethylformamide dimethylacetal (153 mL, 1078 mmol, Aldrich) was refluxed overnight. The reaction mixture was then cooled, concentrated under reduced pressure and the residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-5% methanol in dichloromethane) to provide 6.9 g (99%) of the title compound. MS (ESI+) m/z 195 (M+H)+.

Aufarbeitung

  1. temperaturewas refluxed overnight
  2. temperatureThe reaction mixture was then cooled
  3. concentrationconcentrated under reduced pressure
  4. customthe residue was purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-ab140c35fa8047ea8097a7d65dc39f06
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08492371B2

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