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Sodium Hydroxide → HCID 70124887, Verbindung

HRID 1596343
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1596343
[CH:1]12[CH2:9][CH2:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][N:3]([C:10]([CH2:12][N:13]1[C:19]3[C:20]([CH3:24])=[CH:21][CH:22]=[CH:23][C:18]=3[C:17]([CH2:25][O:26]C(=O)C)=[N:16][CH:15]([NH:30][C:31]([O:33][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)=[O:32])[C:14]1=[O:41])=[O:11])[CH2:2]2.[OH-].[Na+]>C(O)C>[CH:5]12[CH2:8][CH2:9][CH:1]([CH2:7][CH2:6]1)[CH2:2][N:3]([C:10]([CH2:12][N:13]1[C:19]3[C:20]([CH3:24])=[CH:21][CH:22]=[CH:23][C:18]=3[C:17]([CH2:25][OH:26])=[N:16][CH:15]([NH:30][C:31]([O:33][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)=[O:32])[C:14]1=[O:41])=[O:11])[CH2:4]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 54535690HCID 54535690, Verbindung

Produkt 1

HCID 70124887HCID 70124887, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of (3RS)-1-[(3-azabicyclo[3.2.2]non-3-yl)carbonylmethyl]-3-benzyloxycarbonylamino-5-acetoxymethyl-9-methyl-2,3-dihydro-1H-1,4-benzodiazepin-2-one (1.9 g) in ethanol (40 ml) was added 1N-sodium hydroxide solution (7 ml) under stirring at ambient temperature. The mixture was stirred for 20 minutes under the same conditions. After removal of the solvent water was added into the mixture, which was adjusted to pH 4 with a diluted hydrochloric acid and extracted with ethyl acetate twice. The combined extract was washed with water and dried over magnesium sulfate. Removal of the solvent gave (3RS)-1-[(3-azabicyclo[3.2.2]non-3-yl)carbonylmethyl]-3-benzyloxycarbonylamino-5-hydroxymethyl-9-methyl-2,3-dihydro-1H-1,4-benzodiazepin-2-one as an amorphous mass (1.68 g, 95.3%).

Aufarbeitung

  1. stirringThe mixture was stirred for 20 minutes under the same conditions
  2. customAfter removal of the solvent water
  3. additionwas added into the mixture, which
  4. extractionextracted with ethyl acetate twice
  5. extractionThe combined extract
  6. washwas washed with water
  7. dry with materialdried over magnesium sulfate
  8. customRemoval of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-f93f801e48f84000a1786a120b3acd6c
Quelldatensatz
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06291452B1

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