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Ethanol → HCID 23676786, Verbindung

HRID 1492715
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1492715
Cl[C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([C:12]([F:15])([F:14])[F:13])[N:3]=1.[S:16]([O-:19])([OH:18])=[O:17].[Na+:20].C(O)C>O>[F:9][C:8]([F:11])([F:10])[C:6]1[CH:5]=[C:4]([C:12]([F:15])([F:14])[F:13])[N:3]=[C:2]([S:16]([O-:19])(=[O:18])=[O:17])[CH:7]=1.[Na+:20]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 702EthanolHCID 147362352-Chloro-4,6-bis(trifluoromethyl)pyridineHCID 23665763Sodium Bisulfite

Produkt 1

HCID 23676786HCID 23676786, VerbindungAusbeute 66,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 2-chloro-4,6-bis(trifluoromethyl)pyridine (2.50 g, 10 mmol), sodium hydrogen sulfite (4.2 g, 40 mmol), ethanol (40 ml) and water (40 ml) was heated under reflux for 96.5 hours. The reaction mixture was evaporated to dryness under reduced pressure. To the residue, conc. hydrochloric acid was added and the mixture was again evaporated to dryness. The residued was extracted with methanol, and a methanol phase was filtered. The filtrate was evaporated to dryness under reduced pressure to obtain sodium 4,6-bis(trifluoromethyl)pyridine-2-sulfonate (2.11 g). Yield, 66%.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 96.5 hours
  3. customThe reaction mixture was evaporated to dryness under reduced pressure
  4. additionTo the residue, conc. hydrochloric acid was added
  5. customthe mixture was again evaporated to dryness
  6. extractionThe residued was extracted with methanol
  7. filtrationa methanol phase was filtered
  8. customThe filtrate was evaporated to dryness under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cda1434a02ab404f8138736b285264a8
Quelldatensatz
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05374732

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