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Lithium hydroxide, monohydrate → 1-[(2'-t-Butoxycarbonylbiphenyl-4-yl)methyl]-4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylic acid

HRID 265045
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 265045
O.[OH-].[Li+].[C:4]([O:8][C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]1[CH:22]=[CH:21][C:20]([CH2:23][N:24]2[C:28]([C:29]([O:31]CC)=[O:30])=[C:27]([C:34]([OH:37])([CH3:36])[CH3:35])[N:26]=[C:25]2[CH2:38][CH2:39][CH3:40])=[CH:19][CH:18]=1)=[O:10])([CH3:7])([CH3:6])[CH3:5]>O.O1CCOCC1>[C:4]([O:8][C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]1[CH:22]=[CH:21][C:20]([CH2:23][N:24]2[C:28]([C:29]([OH:31])=[O:30])=[C:27]([C:34]([OH:37])([CH3:36])[CH3:35])[N:26]=[C:25]2[CH2:38][CH2:39][CH3:40])=[CH:19][CH:18]=1)=[O:10])([CH3:7])([CH3:6])[CH3:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 10625404Ethyl 1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylate

Produkt 1

HCID 106244931-[(2'-t-Butoxycarbonylbiphenyl-4-yl)methyl]-4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylic acidAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 31275
1,4-Dioxane
Lösungsmittel

Versuchsvorschrift

A solution of 4.8 g of lithium hydroxide monohydrate in 100 ml of water was added to a solution of 11.6 g of ethyl 1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylate [prepared as described in step (a) above] in 60 ml of dioxane, and the resulting mixture was stirred at room temperature for 16 hours. The dioxane was removed by distillation under reduced pressure, and then the concentrate was mixed with ice-water and with ethyl acetate, after which 114 ml of 1N aqueous hydrochloric acid were added. The ethyl acetate layer was separated, dried over anhydrous magnesium sulfate and freed from the solvent by distillation under reduced pressure. The crystalline residue was triturated in diisopropyl ether and collected by filtration co give 9.09 g of the title compound, melting at 155°-157° C.

Aufarbeitung

  1. customThe dioxane was removed by distillation under reduced pressure
  2. additionthe concentrate was mixed with ice-water and with ethyl acetate
  3. additionafter which 114 ml of 1N aqueous hydrochloric acid were added
  4. customThe ethyl acetate layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationfreed from the solvent by distillation under reduced pressure
  7. customThe crystalline residue was triturated in diisopropyl ether
  8. filtrationcollected by filtration co

Quellen und Nachweise

ORD-Eintrag
ord-07bee51ef3b945648ed758061c64e391
Quelldatensatz
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05646171

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