2-Butyl-6-(1-hydroxyethyl)-3-[[2'-[1-(triphenylmethyl)-1H-tetrazol-5-yl][1,1'-biphenyl]-4-yl]methyl]-4(3H)-quinazolinone → HCID 178441465, Verbindung

HRID 1654147Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1654147
[CH2:1]([C:5]1[N:14]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[C:28]3[N:32](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:31]=[N:30][N:29]=3)=[CH:18][CH:17]=2)[C:13](=[O:52])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([CH:53]([OH:55])[CH3:54])[CH:11]=2)[N:6]=1)[CH2:2][CH2:3][CH3:4]>CC(C)=O.O.Cl>[CH2:1]([C:5]1[N:14]([CH2:15][C:16]2[CH:17]=[CH:18][C:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[C:28]3[NH:29][N:30]=[N:31][N:32]=3)=[CH:20][CH:21]=2)[C:13](=[O:52])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([CH:53]([OH:55])[CH3:54])[CH:11]=2)[N:6]=1)[CH2:2][CH2:3][CH3:4]

Komponenten

4

Edukt 1

HCID 200793502-Butyl-6-(1-hydroxyethyl)-3-[[2'-[1-(triphenylmethyl)-1H-tetrazol-5-yl][1,1'-biphenyl]-4-yl]methyl]-4(3H)-quinazolinone

Produkt 1

HCID 178441465HCID 178441465, VerbindungAusbeute 68.818,602 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidKatalysatorHCID 18366337Propan-2-one--water (1/1)Lösungsmittel

Versuchsvorschrift

To a suspension of 2.00 g of 2-butyl-6-(1-hydroxyethyl)-3-[[2'-[1-(triphenylmethyl)-1H-tetrazol-5-yl][1,1'-biphenyl]-4-yl]methyl]-4(3H)-quinazolinone in 70 ml of 3:1 acetone-water is added one drop of 5% aqueous hydrochloric acid solution. The mixture is then heated at reflux for 16 hours. After cooling, the reaction mixture is concentrated in vacuo and the residue purified by flash chromatography on silica gel by elution with 9:1 chloroform-methanol to afford 0,915 g of the desired product as a white solid, m.p. 146°-147° C.

Aufarbeitung

  1. temperatureThe mixture is then heated
  2. temperatureat reflux for 16 hours
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture is concentrated in vacuo
  5. customthe residue purified by flash chromatography on silica gel by elution with 9:1 chloroform-methanol

Quellen und Nachweise

ORD-Eintrag
ord-797a7c79fa6044b586f61a5d2b59204d
Quelldatensatz
uspto-grants-1995_04
Patentnummer
US05405849

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