Ammonium Chloride → HCID 86650697, Verbindung
Reaktionsgleichung
[F:1][C:2]1[CH:27]=[C:26]([N+:28]([O-])=O)[CH:25]=[CH:24][C:3]=1[O:4][C:5]1[C:14]2[C:9](=[CH:10][C:11]([O:22][CH3:23])=[C:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH:13]=2)[N:8]=[CH:7][CH:6]=1.[Cl-].[NH4+]>O.C(O)C.[Fe]>[NH2:28][C:26]1[CH:25]=[CH:24][C:3]([O:4][C:5]2[C:14]3[C:9](=[CH:10][C:11]([O:22][CH3:23])=[C:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH:13]=3)[N:8]=[CH:7][CH:6]=2)=[C:2]([F:1])[CH:27]=1Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
Compound 1b (400 mg) was dissolved in a water-ethanol (1:1) mixture (10 mL), and iron powder (1.0 g) and ammonium chloride (1.0 g) were added thereto, followed by stirring at 80° C. for 2 hours. The reaction mixture was filtered through Celite to thereby remove iron powder, and water (100 mL) was added to the filtrate, followed by extraction with ethyl acetate (50 mL). The organic phase was washed with saturated brine (100 mL) and dried over sodium sulfate, followed by concentration under reduced pressure, to thereby yield compound 1c (335 mg, yield: 93%).
Aufarbeitung
- additionwere added
- filtrationThe reaction mixture was filtered through Celite to thereby remove iron powder, and water (100 mL)
- additionwas added to the filtrate
- extractionfollowed by extraction with ethyl acetate (50 mL)
- washThe organic phase was washed with saturated brine (100 mL)
- dry with materialdried over sodium sulfate
- concentrationfollowed by concentration under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-0d21da34e8b747d3a19befdc562a65fa
- Quelldatensatz
- uspto-grants-2012_11
- Patentnummer
- US08304427B2
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