Sodium Hydroxide → HCID 86722243, Verbindung

HRID 869398Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 869398
[C:1]([C:4]1[O:5][C:6]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([Cl:16])[C:7]=2[C:8]=1[NH2:9])(=[O:3])[CH3:2].[CH:17]([C:19]1[N:20]=[C:21]([NH:24][C:25](=[O:29])[CH:26]([CH3:28])[CH3:27])[S:22][CH:23]=1)=O.[OH-].[Na+]>C1COCC1>[NH2:9][C:8]1[C:7]2[C:10]([Cl:16])=[C:11]([O:14][CH3:15])[CH:12]=[CH:13][C:6]=2[O:5][C:4]=1[C:1](=[O:3])[CH:2]=[CH:17][C:19]1[N:20]=[C:21]([NH:24][C:25](=[O:29])[CH:26]([CH3:27])[CH3:28])[S:22][CH:23]=1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 21914786HCID 21914786, VerbindungHCID 86722235HCID 86722235, Verbindung

Produkt 1

HCID 86722243HCID 86722243, VerbindungAusbeute 59,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

7G (2.5 g, 10.4 mmol) was dissolved in THF (25 mL). To the solution was added 11D (2.4 g, 1.2 eq, 12.5 mmol), followed by crushed NaOH powder (0.8 g, 2 eq, 20.8 mmol). The reaction mixture was stirred at room temperature for about 1 hour and the solution was getting darker. After reaction completed, the mixture was poured into ice-water under stirring. The solids were collected by filtration, dried and purified by column chromatography on silica gel to give 2.6 g of pure product 11E.

Aufarbeitung

  1. customAfter reaction
  2. stirringunder stirring
  3. filtrationThe solids were collected by filtration
  4. customdried
  5. custompurified by column chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-eb61d014c8b34da986470282e432c83f
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969373B2

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