Hydrochloric Acid → 3-(3-(((7S)-3,4-dimethoxy-7-bicyclo(4.2.0)octa-1,3,5-trienyl)methylamino)propyl)-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepin-4-one;hydrochloride

HRID 423131Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 423131
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C@@H:7]([CH2:13][NH:14][CH2:15][CH2:16][CH2:17][N:18]1[C:24](=[O:25])[CH2:23][C:22]3[CH:26]=[C:27]([O:32][CH3:33])[C:28]([O:30][CH3:31])=[CH:29][C:21]=3[CH2:20][CH2:19]1)[CH2:6]2.[ClH:34]>C(#N)C.C(OCC)C>[ClH:34].[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C@@H:7]([CH2:13][NH:14][CH2:15][CH2:16][CH2:17][N:18]1[C:24](=[O:25])[CH2:23][C:22]3[CH:26]=[C:27]([O:32][CH3:33])[C:28]([O:30][CH3:31])=[CH:29][C:21]=3[CH2:20][CH2:19]1)[CH2:6]2

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 10389261N-Demethylivabradine

Produkt 1

HCID 666726993-(3-(((7S)-3,4-dimethoxy-7-bicyclo(4.2.0)octa-1,3,5-trienyl)methylamino)propyl)-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepin-4-one;hydrochlorideAusbeute 72,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

300 mg (0.65 mmol) of the amine obtained in Example 2, Step 2, are dissolved in 10 mL of acetonitrile. To the resulting solution there is added 0.65 mL (1.3 mmol, 2 equivalents) of 2M hydrochloric acid solution in diethyl ether. Stirring is carried out at 25° C. for 15 minutes, and then evaporation to dryness. The product is crystallised from 20 mL of acetone. The solid is filtered off and dried. 230 mg of white crystals are obtained.

Aufarbeitung

  1. customevaporation to dryness
  2. customThe product is crystallised from 20 mL of acetone
  3. filtrationThe solid is filtered off
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2d9610d533be42abacb334f404b541fb
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08101747B2

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