Nitric Acid → HCID 56763846, Verbindung

HRID 605310Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 605310
[N+:1]([O-:4])(O)=[O:2].[CH2:5]([O:7][C:8]([C:10]1[S:11][C:12]([Cl:15])=[CH:13][CH:14]=1)=[O:9])[CH3:6]>>[CH2:5]([O:7][C:8]([C:10]1[S:11][C:12]([Cl:15])=[C:13]([N+:1]([O-:4])=[O:2])[CH:14]=1)=[O:9])[CH3:6]

Komponenten

3

Edukt 2

HCID 944Nitric AcidHCID 521808Ethyl 5-chlorothiophene-2-carboxylate

Produkt 1

HCID 56763846HCID 56763846, VerbindungAusbeute 55 %

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

A solution of fuming nitric acid (75 mL) was cooled to 10° C. followed by the addition of 5-chloro-thiophene-2-carboxylic acid ethyl ester (15 g, 78.7 mmol). The resulting mixture was stirred for 30 minutes at 10° C. followed by the addition of ice water. The solution was then extracted with ethyl acetate and dried, then concentrated under vacuum and purified by column chromatography using silica gel to provide 10.29 g (55%) of the title product.

Aufarbeitung

  1. extractionThe solution was then extracted with ethyl acetate
  2. customdried
  3. concentrationconcentrated under vacuum
  4. custompurified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-ab80c8d83b084772a16961669b11eb2b
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07910595B2

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