Hydrochloric Acid → 1-[2-Fluoro-4-(2-{[4-(4-methylpiperazin-1-yl)piperidine-1-carbonyl]amino}piperidin-4-yloxy)phenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester trihydrochloride

HRID 1712668Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1712668
[CH2:1]([O:8][C:9]([C:11]1([C:14](=[O:46])[NH:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH:23]3[CH2:28][CH2:27][NH:26][CH:25]([NH:29][C:30]([N:32]4[CH2:37][CH2:36][CH:35]([N:38]5[CH2:43][CH2:42][N:41]([CH3:44])[CH2:40][CH2:39]5)[CH2:34][CH2:33]4)=[O:31])[CH2:24]3)=[CH:18][C:17]=2[F:45])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:47]>C(OCC)(=O)C>[ClH:47].[ClH:47].[ClH:47].[CH2:1]([O:8][C:9]([C:11]1([C:14](=[O:46])[NH:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH:23]3[CH2:28][CH2:27][NH:26][CH:25]([NH:29][C:30]([N:32]4[CH2:37][CH2:36][CH:35]([N:38]5[CH2:39][CH2:40][N:41]([CH3:44])[CH2:42][CH2:43]5)[CH2:34][CH2:33]4)=[O:31])[CH2:24]3)=[CH:18][C:17]=2[F:45])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 68496027HCID 68496027, Verbindung

Produkt 1

HCID 684981621-[2-Fluoro-4-(2-{[4-(4-methylpiperazin-1-yl)piperidine-1-carbonyl]amino}piperidin-4-yloxy)phenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester trihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

1-[2-Fluoro-4-(2-{[4-(4-methylpiperazin-1-yl)piperidine-1-carbonyl]amino}piperidin-4-yloxy)phenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester (189 mg) was dissolved in ethyl acetate (6 ml), and 4N hydrochloric acid in ethyl acetate (0.3 ml) was added. The resultant mixture was concentrated under reduced pressure, and methanol (0.5 ml) and ethyl acetate (4 ml) was added. The precipitate obtained by filtration was hygroscopic, thus it was collected using methanol (10 ml). The collected solution was again concentrated under reduced pressure, and methanol (0.5 ml) and tert-butyl methyl ether (4 ml) was added. The precipitate was filtered to give the title compound (102 mg).

Aufarbeitung

  1. concentrationThe resultant mixture was concentrated under reduced pressure, and methanol (0.5 ml) and ethyl acetate (4 ml)
  2. additionwas added
  3. customThe precipitate obtained by filtration
  4. customthus it was collected
  5. concentrationThe collected solution was again concentrated under reduced pressure, and methanol (0.5 ml) and tert-butyl methyl ether (4 ml)
  6. additionwas added
  7. filtrationThe precipitate was filtered

Quellen und Nachweise

ORD-Eintrag
ord-43c58f0ff08b4ee7afdbf314b16e1f31
Quelldatensatz
uspto-grants-2010_09
Patentnummer
US07790885B2

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