Hydrochloric Acid → HCID 178519320, Verbindung

HRID 82026Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 82026
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][C:37]([Cl:40])=[CH:36][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.O1CCOCC1>CO>[Cl:40][C:37]1[CH:36]=[CH:35][C:34](/[CH:33]=[CH:32]/[C:31]2[C:17]3[C:18](=[N:19][C:20]([C:22]4[CH:23]=[CH:24][C:25]([OH:28])=[CH:26][CH:27]=4)=[CH:21][C:16]=3[C:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)=[O:15])[NH:29][N:30]=2)=[CH:39][CH:38]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 1363594974-[3-[(E)-2-(4-chloro-phenyl)-vinyl]-6-(4-hydroxy-phenyl)-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carbonyl]-piperazine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 178519320HCID 178519320, VerbindungAusbeute 95,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 4-[3-[(E)-2-(4-chloro-phenyl)-vinyl]-6-(4-hydroxy-phenyl)-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carbonyl]-piperazine-1-carboxylic acid tert-butyl ester (1.32 g, 2.05 mmol) in dry methanol (20 ml) was added 4N HCl in dioxane (5.1 ml, 20 mmol). The reaction mixture was heated to reflux for 30 minutes then cooled to room temperature and filtered. The precipitate was isolated and dried to afford a chlorhydrate salt of the title compound as an orange solid (0.9 g, 90%).

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 30 minutes
  3. filtrationfiltered
  4. customThe precipitate was isolated
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-38aca937d29a460f95dbc812b145b472
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846712B2

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