Hydrogen Peroxide → 2-Carboxyphenoxathiin-10-oxide

HRID 372487

Reaktionsgleichung

Reaktionsgleichung von HRID 372487
[CH:1]1[C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[O:6][C:5]=2[CH:4]=[CH:3][C:2]=1[C:15]([OH:17])=[O:16].[OH:18]O>C(O)C>[C:15]([C:2]1[CH:3]=[CH:4][C:5]2[O:6][C:7]3[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=3)[S:13](=[O:18])[C:14]=2[CH:1]=1)([OH:17])=[O:16]

Komponenten

4

Edukt 2

HCID 784Hydrogen Peroxide2×HCID 8200622-Phenoxathiincarboxylic acid

Produkt 1

HCID 203277292-Carboxyphenoxathiin-10-oxide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Phenoxathiin-2-carboxylic acid (0.61g) was dissolved in refluxing absolute ethanol (40 ml) and 30% w/v hydrogen peroxide solution (1.50 ml) added. Reflux was maintained for 2 hours, more 30% w/v hydrogen peroxide solution (1.00 ml.) added, and reflux continued for 17 hours. The solution was evaporated to low volume, and the product crystallised out. The solid was filtered, washed and dried to give 2-carboxyphenoxathiin-10-oxide m.p. 223° C. Recrystallisation from absolute ethanol raised the melting point to 237° C.

Aufarbeitung

  1. additionadded
  2. temperatureReflux
  3. temperaturewas maintained for 2 hours
  4. additionadded
  5. temperaturereflux
  6. customThe solution was evaporated to low volume
  7. customthe product crystallised out
  8. filtrationThe solid was filtered
  9. washwashed
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-80a36d2874b643b1b071bb17972b06a1
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04091108

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