Hydrochloric Acid → 2-Phenoxathiincarboxylic acid

HRID 2398772

Reaktionsgleichung

Reaktionsgleichung von HRID 2398772
[C:1]([C:4]1[CH:17]=[CH:16][C:15]2[O:14][C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[S:7][C:6]=2[CH:5]=1)(=[O:3])C.Cl[O-:19].[Na+].[OH-].[Na+].Cl>O1CCOCC1>[CH:5]1[C:6]2[S:7][C:8]3[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=3)[O:14][C:15]=2[CH:16]=[CH:17][C:4]=1[C:1]([OH:3])=[O:19]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 5151742-AcetylphenoxathiinHCID 23665760Sodium Hypochlorite

Produkt 1

HCID 8200622-Phenoxathiincarboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of 2-acetylphenoxathiin (4.80 g), sodium hypochlorite solution (95 ml; 5.7% available chlorine), 4% sodium hydroxide solution (100 ml) and dioxan (100 ml) was mechanically stirred on the steam bath for 5 hrs. The solution was poured on to ice and excess hydrochloric acid with stirring. The white precipitate was filtered off and dissolved in hot 4% sodium hydroxide solution (40 ml) and filtered. The sodium salt of the required acid crystallised from the filtrate on cooling and was filtered off, dissolved in boiling water, and the acid precipitated by addition of excess hydrochloric acid. It was filtered off and recrystallised from acetic acid, m.p. 253° C.

Aufarbeitung

  1. stirringwith stirring
  2. filtrationThe white precipitate was filtered off
  3. dissolutiondissolved in hot 4% sodium hydroxide solution (40 ml)
  4. filtrationfiltered
  5. customThe sodium salt of the required acid crystallised from the filtrate
  6. temperatureon cooling
  7. filtrationwas filtered off
  8. dissolutiondissolved
  9. customthe acid precipitated by addition of excess hydrochloric acid
  10. filtrationIt was filtered off
  11. customrecrystallised from acetic acid, m.p. 253° C.

Quellen und Nachweise

ORD-Eintrag
ord-301c0806171e4a94b57625cff7e4d71f
Quelldatensatz
uspto-grants-1977_05
Patentnummer
US04025635

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