Potassium Nitrate → 4,5-dinitro-2-ethoxy-benzoic Acid

HRID 1012124

Reaktionsgleichung

Reaktionsgleichung von HRID 1012124
[N+:1]([O-])([O-:3])=[O:2].[K+].[CH2:6]([O:8][C:9]1[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:10]=1[C:11]([OH:13])=[O:12])[CH3:7]>S(=O)(=O)(O)O>[N+:18]([C:16]1[C:15]([N+:1]([O-:3])=[O:2])=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[C:9]([O:8][CH2:6][CH3:7])[CH:17]=1)([O-:20])=[O:19]

Komponenten

4

Edukt 2

HCID 24434Potassium NitrateHCID 27363472-Ethoxy-4-nitrobenzoic acid

Produkt 1

HCID 858173894,5-dinitro-2-ethoxy-benzoic AcidAusbeute 87,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

To a mixture of potassium nitrate (4.80 g, 47.4 mmol) in concentrated sulphuric acid (20 mL) was added portion-wise at 0° C. 2-ethoxy-4-nitrobenzoic acid (4.00 g, 19.0 mmol). The mixture was stirred at 0° C.-r.t. for 3 h, then poured onto ice (120 mL) and stirred for a further 1 h. The precipitate formed was collected by filtration, washing with water, and dried through azeotrope with toluene to give the title compound (4.28 g) as a white solid. 1H NMR (300 MHz, DMSO-d6) δ 8.50 (s, 1H), 7.95 (s, 1H), 4.35 (q, 2H), 1.35 (t, 3H).

Aufarbeitung

  1. additionwas added portion-wise at 0° C
  2. additionpoured onto ice (120 mL)
  3. stirringstirred for a further 1 h
  4. customThe precipitate formed
  5. filtrationwas collected by filtration
  6. washwashing with water
  7. dry with materialdried through azeotrope with toluene

Quellen und Nachweise

ORD-Eintrag
ord-b8676b560d514569898e9a9f44748f2b
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977477B2

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