Methanol → HCID 60451708, Verbindung

HRID 417303Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 417303
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[C:9]([OH:11])=[O:10])[CH2:2][CH2:3][CH3:4].OS(O)(=O)=O.[CH3:23]O>>[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[C:9]([O:11][CH3:23])=[O:10])[CH2:2][CH2:3][CH3:4]

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 2535313-Butoxy-4-nitrobenzoic acid

Produkt 1

HCID 60451708HCID 60451708, VerbindungAusbeute 95 %

Versuchsvorschrift

To a solution of 3-butoxy-4-nitrobenzoic acid (City Chemicals) (2.5 g, 10.5 mmol) in methanol (10 mL) were added concentrated H2SO4 (1 g, 10.5 mmol). The reaction mixture was heated at reluxing for 2 h. The mixture was concentrated. The residue was partitioned between ethyl acetate and water. The organic layer was separated, and aqueous layer was extracted with ethyl acetate twice. The combined organic extract was washed with water, aqueous saturated NaHCO3 solution, brine, dried over MgSO4, and concentrated to give methyl 3-butoxy-4-nitrobenzoate as a brown oil (2.5 g, 95%).

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. concentrationThe mixture was concentrated
  3. customThe residue was partitioned between ethyl acetate and water
  4. customThe organic layer was separated
  5. extractionaqueous layer was extracted with ethyl acetate twice
  6. extractionThe combined organic extract
  7. washwas washed with water, aqueous saturated NaHCO3 solution, brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-3aeefc76e4004d3997b01eafcac4050b
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08088815B2

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