Nitric Acid → Methyl 7-Nitro-1,4-benzodioxane-6-carboxylate

HRID 1579241Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1579241
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]2[O:10][CH2:11][CH2:12][O:13][C:6]=2[CH:5]=1.[N+:15]([O-])([OH:17])=[O:16]>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:14])[C:4]1[C:9]([N+:15]([O-:17])=[O:16])=[CH:8][C:7]2[O:10][CH2:11][CH2:12][O:13][C:6]=2[CH:5]=1

Komponenten

4

Edukt 2

HCID 944Nitric AcidHCID 3802178Methyl 2,3-dihydro-1,4-benzodioxine-6-carboxylate

Produkt 1

HCID 10537941Methyl 7-Nitro-1,4-benzodioxane-6-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

To a solution of 5.0 g. of 3,4-ethylenedioxybenzoic acid methyl ester in 5.0 mls. of glacial acetic acid is added dropwise 5.0 mls. of 70% nitric acid at 50°-60°C. After addition the reaction mixture is kept at 55°C. for one hour, then cooled and 50 mls. of ice water added. The resulting precipitate is recovered by filtering, water washed and dried to obtain 6-nitro-3,4-ethylenedioxybenzoic acid methyl ester, m.p. 115°-118°C.

Aufarbeitung

  1. customat 50°-60°C
  2. additionAfter addition the reaction mixture
  3. temperaturecooled
  4. customThe resulting precipitate is recovered
  5. filtrationby filtering
  6. washwater washed
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-1fad555a79854f74bb5f8c06a05248b2
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03931179

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