1,4-Dioxane hydrochloride → Hydrochloric Acid

HRID 11849Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 11849
C([N:8]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]([NH:25][C@@H:26]([CH2:30][CH2:31][CH2:32][NH:33][CH:34]2[C:43]3[N:42]=[CH:41][CH:40]=[CH:39][C:38]=3[CH2:37][CH2:36][CH2:35]2)[C:27]([OH:29])=[O:28])=[O:24])=[CH:19][N:18]=1)[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1)(OC(C)(C)C)=O.[ClH:44].O1CCOCC1>CO>[ClH:44].[N:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[CH2:9][NH:8][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]([NH:25][C@@H:26]([CH2:30][CH2:31][CH2:32][NH:33][CH:34]2[C:43]3[N:42]=[CH:41][CH:40]=[CH:39][C:38]=3[CH2:37][CH2:36][CH2:35]2)[C:27]([OH:29])=[O:28])=[O:24])=[CH:19][N:18]=1

Komponenten

5

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 21043726(2S)-2-(2-(N-Boc-N-2-picolylaminomethyl)pyridin-5-ylcarbonyl)amino-5-(5,6,7,8-tetrahydroquinolin-8-yl)aminovaleric Acid

Produkt 2

HCID 313Hydrochloric AcidHCID 69638179(2S)-2-(2-(N-2-picolylaminomethyl)pyridin-5-ylcarbonyl)amino-5-((5,6,7,8-tetrahydroquinolin-8-yl)amino)valeric Acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

The compound obtained in Example 12-5 (26.8 mg) was dissolved in methanol (0.5 ml), and 4 mol/l hydrochloric acid/dioxane solution (0.5 ml) was added. The mixture was stirred for 4.5 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5). The obtained product was added with an aqueous solution of hydrochloric acid and concebtrated, and then azeotropically distilled with water. The resulting solid was washed with ether to obtain a hydrochloride of the title compound (25.8 mg) as a white solid.

Aufarbeitung

  1. customAfter the reaction
  2. customthe solvent was removed by distillation
  3. customThe residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5)
  4. additionThe obtained product was added with an aqueous solution of hydrochloric acid
  5. distillationazeotropically distilled with water
  6. washThe resulting solid was washed with ether

Quellen und Nachweise

ORD-Eintrag
ord-ba3b184e2c9341639bd6d7c29b775726
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07098215B2

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