4-Benzoyl-2-butyl-5-cyano-1-tritylimidazole → HCID 178441735, Verbindung

HRID 53022Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 53022
[C:1]([C:9]1[N:10]=[C:11]([CH2:35][CH2:36][CH2:37][CH3:38])[N:12](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[C:13]=1[C:14]#[N:15])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)(=O)C>[C:1]([C:9]1[N:10]=[C:11]([CH2:35][CH2:36][CH2:37][CH3:38])[NH:12][C:13]=1[C:14]#[N:15])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

3

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A suspension of 10.3 g of 4-benzoyl-2-butyl-5-cyano-1-tritylimidazole [prepared as described in step (i) above] in 80% v/v aqueous acetic acid was stirred at 60° C. for 5 hours. At the end of this time, the solution thus obtained was concentrated by evaporation under reduced pressure, and the concentrate was purified by column chromatography through silica gel, using a 2:1 by volume mixture of hexane and ethyl acetate as the eluent. The resulting oily product was dissolved in carbon tetrachloride and the solution was allowed to stand at room temperature, to precipitate crystals, which were collected by filtration to give 4.46 g of the title compound, melting at 121°-122° C.

Aufarbeitung

  1. customAt the end of this time, the solution thus obtained
  2. concentrationwas concentrated by evaporation under reduced pressure
  3. customthe concentrate was purified by column chromatography through silica gel
  4. additionby volume mixture of hexane and ethyl acetate as the eluent
  5. dissolutionThe resulting oily product was dissolved in carbon tetrachloride
  6. customto stand at room temperature
  7. customto precipitate crystals, which
  8. filtrationwere collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-41c65f04e1cd470d9c1b2ead189201e9
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05616599

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