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Sulfuric Acid → HCID 22457397, Verbindung

HRID 2184630
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2184630
[N+:1]([C:4]1[CH:5]=[C:6]([C:13]([OH:15])=[O:14])[C:7](=[CH:11][CH:12]=1)[C:8]([OH:10])=[O:9])([O-:3])=[O:2].S(=O)(=O)(O)O>C(O)C>[N+:1]([C:4]1[CH:5]=[C:6]([C:13]([O:15][CH2:13][CH2:6][CH2:7][CH3:8])=[O:14])[C:7](=[CH:11][CH:12]=1)[C:8]([O:10][CH2:5][CH2:4][CH2:12][CH3:11])=[O:9])([O-:3])=[O:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 1118Sulfuric AcidHCID 691211,2-Benzenedicarboxylic acid, 4-nitro-

Produkt 1

HCID 22457397HCID 22457397, VerbindungAusbeute 136,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

4-nitrophthalic acid (2.0 g, 9.5 mmol) was dissolved in 30 ml of absolute ethanol and then 0.3 ml of concentrated sulfuric acid was added. The mixture was heated at 120° C. for 24 hours, and the solvent was evaporated under reduced pressure. The oily residue was dissolved in diethyl ether and washed three times with water and once with 10% Na2CO3 solution. The ether solution was dried over anhydrous sodium sulfate. After evaporation of the solvent, a light yellow crude solid was obtained. The crude product was purified by silica gel column chromatography (n-hexane: acetic acid =10:1) to give 2.1 g (68.4%) of di-n-butyl 4-nitrophthalate (compound 403).

Aufarbeitung

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionThe oily residue was dissolved in diethyl ether
  3. washwashed three times with water
  4. dry with materialThe ether solution was dried over anhydrous sodium sulfate
  5. customAfter evaporation of the solvent
  6. customa light yellow crude solid was obtained
  7. customThe crude product was purified by silica gel column chromatography (n-hexane: acetic acid =10:1)

Quellen und Nachweise

ORD-Eintrag
ord-128edfc196634d60801854f711646ac2
Quelldatensatz
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06399318B1

Notizen zur Reaktion

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