Hydrochloric Acid → HCID 178519321, Verbindung

HRID 82047

Reaktionsgleichung

Reaktionsgleichung von HRID 82047
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[C:17]3[C:31](/[CH:32]=[CH:33]/[C:34]4[CH:39]=[CH:38][CH:37]=[C:36]([N:40]5[CH2:44][CH2:43][CH2:42][C:41]5=[O:45])[CH:35]=4)=[N:30][N:29](C4CCCCO4)[C:18]=3[N:19]=[C:20]([C:22]3[CH:27]=[CH:26][C:25]([OH:28])=[CH:24][CH:23]=3)[CH:21]=2)=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.C(OCC)C>CO.O1CCOCC1>[OH:28][C:25]1[CH:24]=[CH:23][C:22]([C:20]2[N:19]=[C:18]3[NH:29][N:30]=[C:31](/[CH:32]=[CH:33]/[C:34]4[CH:35]=[C:36]([N:40]5[CH2:44][CH2:43][CH2:42][C:41]5=[O:45])[CH:37]=[CH:38][CH:39]=4)[C:17]3=[C:16]([C:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)=[O:15])[CH:21]=2)=[CH:27][CH:26]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 1363595064-[6-(4-Hydroxy-phenyl)-3-{(E)-2-[3-(2-oxo-pyrrolidin-1-yl)-phenyl]-vinyl}-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carbonyl]-piperazine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 178519321HCID 178519321, VerbindungAusbeute 103,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of 4-[6-(4-Hydroxy-phenyl)-3-{(E)-2-[3-(2-oxo-pyrrolidin-1-yl)-phenyl]-vinyl}-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carbonyl]-piperazine-1-carboxylic acid tert-butyl ester (0.246 g, 0.36 mmol) in methanol (5 ml) was added 4N HCl in dioxane (0.9 ml). The reaction mixture was stirred at room temperature for 18 hours, diethyl ether was then added, the resulting precipitated was filtered and washed once with diethyl ether to afford the hydrochloride salt of the title compound (0.19 g, 93%) as an orange solid.

Aufarbeitung

  1. customthe resulting precipitated
  2. filtrationwas filtered
  3. washwashed once with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-bd553274a4454a5692b47b0a45b0e01b
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846712B2

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