Sodium Hydroxide → HCID 178445683, Verbindung

HRID 1992802Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1992802
[C:1]([C@@H:5]1[CH2:10][CH2:9][C@H:8]([NH:11][C:12]([C:14]2[N:18]([CH2:19][C:20]3[CH:29]=[CH:28][C:23]([C:24]([O:26]C)=[O:25])=[CH:22][N:21]=3)[N:17]=[C:16]([C:30]3[CH:35]=[CH:34][C:33]([Cl:36])=[C:32]([Cl:37])[CH:31]=3)[CH:15]=2)=[O:13])[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>C1COCC1.CO>[C:1]([C@@H:5]1[CH2:6][CH2:7][C@H:8]([NH:11][C:12]([C:14]2[N:18]([CH2:19][C:20]3[CH:29]=[CH:28][C:23]([C:24]([OH:26])=[O:25])=[CH:22][N:21]=3)[N:17]=[C:16]([C:30]3[CH:35]=[CH:34][C:33]([Cl:36])=[C:32]([Cl:37])[CH:31]=3)[CH:15]=2)=[O:13])[CH2:9][CH2:10]1)([CH3:4])([CH3:2])[CH3:3]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 178497906HCID 178497906, Verbindung

Produkt 1

HCID 178445683HCID 178445683, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21899815MeOH tetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of the intermediate from step G (isomer B) (0.14 g, 0.24 mmol) in 10 ml of 1:1 THF/MeOH was added 5 N NaOH (1 mL). After stirring the reaction at room temperature for 2 hours, it was concentrated in vacuo. The residue was acidified with 1N HCl (10 ml) and the resulting mixture was extracted with ethyl acetate, dried over anhydrous Na2SO4 filtered and concentrated in vacuo. This material was used in the next step without any further purification.

Aufarbeitung

  1. customthe reaction at room temperature for 2 hours
  2. concentrationit was concentrated in vacuo
  3. extractionthe resulting mixture was extracted with ethyl acetate
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThis material was used in the next step without any further purification

Quellen und Nachweise

ORD-Eintrag
ord-df8d3c8f27c5484386299df76527078d
Quelldatensatz
uspto-grants-2010_01
Patentnummer
US07649009B2

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