Sodium Hydroxide → 1-methoxycarbonyl-7-(4-morpholinophenyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid

HRID 586866Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 586866
[CH3:1][O:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][C:14]([C:16]3[CH:21]=[CH:20][C:19]([N:22]4[CH2:27][CH2:26][O:25][CH2:24][CH2:23]4)=[CH:18][CH:17]=3)=[CH:15][C:10]=2[CH:9]=[C:8]([C:28]([O:30]C)=[O:29])[CH2:7][CH2:6]1)=[O:4].[OH-].[Na+]>CO.C1COCC1>[CH3:1][O:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][C:14]([C:16]3[CH:17]=[CH:18][C:19]([N:22]4[CH2:27][CH2:26][O:25][CH2:24][CH2:23]4)=[CH:20][CH:21]=3)=[CH:15][C:10]=2[CH:9]=[C:8]([C:28]([OH:30])=[O:29])[CH2:7][CH2:6]1)=[O:4]

Komponenten

5

Edukt 2

HCID 14798Sodium Hydroxide2×HCID 22328989HCID 22328989, Verbindung

Produkt 1

HCID 223292091-methoxycarbonyl-7-(4-morpholinophenyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylic acidAusbeute 96,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

In methanol (40 ml) and THF (60 ml) was dissolved methyl 1-methoxycarbonyl-7-(4-morpholinophenyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylate (0.31 g). To the solution was-added 1N sodium hydroxide solution (5 ml), and the mixture was stirred at room temperature overnight. To the mixture was added 1N sodium hydroxide solution (2.5 ml), and the mixture was stirred at room temperature overnight and concentrated. The residue was neutralized with 1N hydrochloric acid, precipitated crystals were filtered and washed with water to give 1-methoxycarbonyl-7-(4-morpholinophenyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid (0.29 g) as colorless crystals.

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature overnight
  2. concentrationconcentrated
  3. customprecipitated crystals
  4. filtrationwere filtered
  5. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-c47cf545b6d744548bb8ecb121bde0dd
Quelldatensatz
uspto-grants-2005_08
Patentnummer
US06936602B1

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