Methanol → Methyl 4-chloro-3,5-dinitrobenzoate

HRID 236939

Reaktionsgleichung

Reaktionsgleichung von HRID 236939
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].[CH3:17]O>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:3]([N+:14]([O-:16])=[O:15])=[CH:4][C:5]([C:6]([O:8][CH3:17])=[O:7])=[CH:9][C:10]=1[N+:11]([O-:13])=[O:12]

Komponenten

4

Edukt 2

HCID 887MethanolHCID 83774-Chloro-3,5-dinitrobenzoic acid

Produkt 1

HCID 96161Methyl 4-chloro-3,5-dinitrobenzoateAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

4-Chloro-3,5-dinitrobenzoic acid (25.0 gm.) is dissolved in a cooled solution of methanol (125 ml.) and concentrated sulfuric acid (3.0 ml.). The reaction mixture is allowed to warm to room temperature and then heated to reflux for 18 hours. The product precipitated as light yellow needles on cooling, which are collected by filtration and washed with 15 ml. of methanol (24.0 gm., m.p. 102°-104.5°). Recrystallization from methanol gives light yellow needles (23.6 g., m.p. 104- 105.5). 89% yield).

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux for 18 hours
  3. customThe product precipitated as light yellow needles
  4. temperatureon cooling
  5. filtrationwhich are collected by filtration
  6. washwashed with 15 ml
  7. customRecrystallization from methanol
  8. customgives light yellow needles (23.6 g., m.p. 104- 105.5)

Quellen und Nachweise

ORD-Eintrag
ord-c33b0a758598405cafca331d6911881a
Quelldatensatz
uspto-grants-1979_06
Patentnummer
US04159278

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