Ethanol → HCID 22929815, Verbindung

HRID 1295953Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1295953
[C:1]([C:5]1[CH:6]=[C:7]([C:16](=[O:18])[CH3:17])[CH:8]=[C:9]([N+:13]([O-])=O)[C:10]=1[O:11][CH3:12])([CH3:4])([CH3:3])[CH3:2].[Cl-].[NH4+].C(O)C.O>[Fe].C(OCC)(=O)C>[NH2:13][C:9]1[CH:8]=[C:7]([C:16](=[O:18])[CH3:17])[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[C:10]=1[O:11][CH3:12]

Komponenten

7

Edukt 4

HCID 702EthanolHCID 962WaterHCID 25517Ammonium ChlorideHCID 589100541-(3-tert-Butyl-4-methoxy-5-nitrophenyl)ethan-1-one

Produkt 1

HCID 22929815HCID 22929815, VerbindungAusbeute 48,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Iron powder (365 g) was added to a mixture of 1-[3-(tert-butyl)-4-methoxy-5-nitrophenyl]-1-ethanone (850 g), ammonium chloride (723 g), ethanol (4 l) and water (1 l) at 70° C. to 80° C. over a period of 1 hour. The reaction mixture was cooled to room temperature and then poured into a mixture of ice water and ethyl acetate and filtered through celite. The organic layer of the mother liquor was washed with brine and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the resulting crystals were filtered off to yield the title compound (362 g) as white crystals.

Aufarbeitung

  1. filtrationfiltered through celite
  2. washThe organic layer of the mother liquor was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. filtrationthe resulting crystals were filtered off

Quellen und Nachweise

ORD-Eintrag
ord-33a2a1170a504d928d28cf91ab1e61c5
Quelldatensatz
uspto-grants-2007_07
Patentnummer
US07244730B2

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