Sodium Hydroxide → HCID 68444484, Verbindung

HRID 2188601Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2188601
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:6]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:5][CH:4]([NH:19][C:20](=[O:32])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:27]([O:29]CC)=[O:28])[C:3]1=[O:33].[OH-].[Na+].[NH4+].[Cl-]>C1COCC1.CO.O>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:6]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:5][CH:4]([NH:19][C:20](=[O:32])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:27]([OH:29])=[O:28])[C:3]1=[O:33]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 59635614HCID 59635614, Verbindung

Produkt 1

HCID 68444484HCID 68444484, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21892291Methanol tetrahydrofuran waterLösungsmittel

Versuchsvorschrift

15 (0.58 g, 1.29 mmol) and NaOH (0.08 g, 1.5 eq) were stirred in a mixture of THF/MeOH/H2O (2 mL each) for 2 h at room temperature. The mixture was treated with a saturated solution of NH4Cl and extracted with AcOEt. Drying (Na2SO4) and removal of the solvent gave 8-(1-methyl-2-oxo-5-phenyl-2,3-dihydro-1H-benzo[e][1,4]diazepin-3-ylamino)-8-oxooctanoic acid in 99% yield as a white solid (m.p. 140-141° C.).

Aufarbeitung

  1. extractionextracted with AcOEt
  2. customDrying
  3. custom(Na2SO4) and removal of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-1cc5ecea4f9a48c8827661c0b35f9326
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08324202B2

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