Hydrochloric Acid → HCID 178480059, Verbindung

HRID 216362Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 216362
Cl.[CH3:2][C:3]([CH3:46])([CH3:45])[CH2:4][C:5]1[N:6]=[C:7]([CH2:29][C:30]([C:33]2[CH:38]=[CH:37][C:36]([C:39]3[CH:40]=[N:41][N:42]([CH3:44])[CH:43]=3)=[CH:35][CH:34]=2)([OH:32])[CH3:31])[N:8](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:9]=1>CO>[CH3:2][C:3]([CH3:46])([CH3:45])[CH2:4][C:5]1[N:6]=[C:7]([CH2:29][C:30]([C:33]2[CH:38]=[CH:37][C:36]([C:39]3[CH:40]=[N:41][N:42]([CH3:44])[CH:43]=3)=[CH:35][CH:34]=2)([OH:32])[CH3:31])[NH:8][CH:9]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 686676631-[4-(2,2-dimethylpropyl)-1-trityl-1H-imidazol-2-yl]-2-[4-(1-methyl-1H-pyrazol-4-yl)phenyl]propan-2-ol

Produkt 1

HCID 178480059HCID 178480059, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Hydrogen chloride (4 M in 1,4-dioxane) (5.25 mL, 21 mmol) was added to an ambient temperature solution of 1-[4-(2,2-dimethylpropyl)-1-trityl-1H-imidazol-2-yl]-2-[4-(1-methyl-1H-pyrazol-4-yl)phenyl]propan-2-ol (250 mg, 0.42 mmol) in methanol (10 mL). After stirring at 70° C. for 1 h, volatiles were removed. The residue was partitioned between diethyl ether and 1 N hydrochloric acid. The aqueous phase was washed with diethyl ether, basified with 2.5 N aqueous sodium hydroxide and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried (sodium sulfate) and concentrated in vacuo to afford the title compound. (M+H) found 339.

Aufarbeitung

  1. customvolatiles were removed
  2. customThe residue was partitioned between diethyl ether and 1 N hydrochloric acid
  3. washThe aqueous phase was washed with diethyl ether
  4. extractionextracted with ethyl acetate
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried (sodium sulfate)
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-eef7da6afb894142967b5ee27be5ba2e
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08193228B2

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