Water → HCID 178470643, Verbindung

HRID 230731

Reaktionsgleichung

Reaktionsgleichung von HRID 230731
S(OS([O-])=O)([O-])=O.[Na+].[Na+].[Cl:10][C:11]1[S:12][C:13]([CH:16]=O)=[CH:14][CH:15]=1.[NH2:18][C:19]1[CH:20]=[C:21]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH:22]=[CH:23][C:24]=1[NH2:25].O>CN1CCCC1=O>[Cl:10][C:11]1[S:12][C:13]([C:16]2[NH:25][C:24]3[CH:23]=[CH:22][C:21]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:20][C:19]=3[N:18]=2)=[CH:14][CH:15]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 24346Disodium disulfiteHCID 817002-Thiophenecarboxaldehyde, 5-chloro-HCID 12986345Ethyl 2-(3,4-diaminophenyl)acetate

Produkt 1

HCID 178470643HCID 178470643, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

3.1 3.89 g (20.5 mmol) of sodium disulfite are added to a solution of 3.00 g (20.5 mmol) of 2-chlorothiophene-5-carbaldehyde and 3.98 g (20.5 mmol) of ethyl 3,4-diaminophenylacetate in 30 ml of 1-methyl-pyrrolidone, and the mixture is stirred at 110° C. for 18 hours. Water is added to the reaction mixture, which is extracted with dichloromethane. The organic phase is dried using sodium sulfate and evaporated, giving ethyl [2-(5-chlorothiophen-2-yl)-1H-benzimidazol-5-yl]acetate as a brown oil (ESI 321), which is employed without further purification for the next reaction.

Aufarbeitung

  1. extractionis extracted with dichloromethane
  2. customThe organic phase is dried
  3. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-007244662b1a4f669932ccf3d84cc4e2
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07566789B2

Verknüpfte Notizen

Wird geladen…