Hydrochloric Acid → HCID 44517481, Verbindung

HRID 877259Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 877259
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[O:18])[N:10]([CH2:19][C:20]3[CH:25]=[CH:24][C:23]([CH:26]([CH:41]4[CH2:45][CH2:44][CH2:43][CH2:42]4)[C:27]([NH:29][CH2:30][C:31]4[CH:36]=[CH:35][C:34]([C:37]([O:39]C)=[O:38])=[CH:33][CH:32]=4)=[O:28])=[CH:22][CH:21]=3)[N:9]=2)=[CH:4][CH:3]=1.[OH-].[Na+].Cl>O1CCOCC1.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[O:18])[N:10]([CH2:19][C:20]3[CH:25]=[CH:24][C:23]([CH:26]([CH:41]4[CH2:45][CH2:44][CH2:43][CH2:42]4)[C:27]([NH:29][CH2:30][C:31]4[CH:32]=[CH:33][C:34]([C:37]([OH:39])=[O:38])=[CH:35][CH:36]=4)=[O:28])=[CH:22][CH:21]=3)[N:9]=2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 58136535HCID 58136535, Verbindung

Produkt 1

HCID 44517481HCID 44517481, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 218864351,4-Dioxane--water (1/1)Lösungsmittel

Versuchsvorschrift

270 mg (0.435 mmol) of methyl 4-({[(4-{[4-(4-chlorophenyl)-1-oxophthalazin-2(1H)-yl]methyl}phenyl)(cyclopentyl)acetyl]amino}methyl)benzenecarboxylate (Example 112A) were dissolved in 10 ml of dioxane/water (3:1 v/v), and 0.652 ml (0.652 mmol) of 1 N aqueous sodium hydroxide solution was added. The mixture was stirred at room temperature overnight. The reaction mixture was then acidified with 1 N hydrochloric acid and extracted repeatedly with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated under reduced pressure. This gave 269 mg of the target compound.

Aufarbeitung

  1. extractionextracted repeatedly with ethyl acetate
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-efa61b8e514346c9bf45c0b36a6fa014
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08987256B2

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