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Hydrochloric Acid → 4-Acetyl-2-butyl-1-[(2'-carboxybiphenyl-4-yl)methyl]-5-cyanoimidazole

HRID 52885
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 52885
[C:1]([C:4]1[N:5]=[C:6]([CH2:31][CH2:32][CH2:33][CH3:34])[N:7]([CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[C:24]([O:26]C(C)(C)C)=[O:25])=[CH:14][CH:13]=2)[C:8]=1[C:9]#[N:10])(=[O:3])[CH3:2].Cl>O1CCOCC1>[C:1]([C:4]1[N:5]=[C:6]([CH2:31][CH2:32][CH2:33][CH3:34])[N:7]([CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[C:24]([OH:26])=[O:25])=[CH:14][CH:13]=2)[C:8]=1[C:9]#[N:10])(=[O:3])[CH3:2]
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Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 190361124-Acetyl-1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-2-butyl-5-cyanoimidazole

Produkt 1

HCID 190361394-Acetyl-2-butyl-1-[(2'-carboxybiphenyl-4-yl)methyl]-5-cyanoimidazoleAusbeute 96,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of 1.3 g of 4-acetyl-1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-2-butyl-5-cyanoimidazole [prepared as described in step (a) above] in 30 ml of a 4N solution of hydrogen chloride in dioxane was allowed to stand overnight at room temperature, after which it was concentrated by evaporation under reduced pressure. The concentrate was purified by column chromatography through silica gel, using a 10:1 by volume mixture of methylene chloride and methanol as the eluent, to give a colorless amorphous solid. The solid was triturated in hexane, collected by filtration and dried, to give 1.1 g of the title compound, melting at above 55° C. (with softening).

Aufarbeitung

  1. concentrationafter which it was concentrated by evaporation under reduced pressure
  2. customThe concentrate was purified by column chromatography through silica gel
  3. additionby volume mixture of methylene chloride and methanol as the eluent
  4. customto give a colorless amorphous solid
  5. customThe solid was triturated in hexane
  6. filtrationcollected by filtration
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-4fc2f5a593784da08f3277db243314fa
Quelldatensatz
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05616599

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