Acetic Acid → HCID 21320318, Verbindung

HRID 262226Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 262226
[CH3:1][S:2][CH2:3][C:4]1[CH:5]=[CH:6][C:7]2[O:11][C:10]([N+:12]([O-:14])=[O:13])=[C:9]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:8]=2[CH:21]=1.C(O)(=[O:24])C.OO.[OH2:28]>>[CH3:1][S:2]([CH2:3][C:4]1[CH:5]=[CH:6][C:7]2[O:11][C:10]([N+:12]([O-:14])=[O:13])=[C:9]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:8]=2[CH:21]=1)(=[O:24])=[O:28]

Komponenten

5

Edukt 4

HCID 176Acetic Acid2×HCID 784Hydrogen PeroxideHCID 962WaterHCID 21320301HCID 21320301, Verbindung

Produkt 1

HCID 21320318HCID 21320318, Verbindung

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

A mixture of 2.8 g. (0.009 mole) of 5-methylthiomethyl-2-nitro-3-phenylbenzofuran and 160 ml. of acetic acid is heated to 40° C., and 2.0 g. (0.018 mole) of hydrogen peroxide in 30 ml. of acetic acid is added dropwise as the temperature rises to 50° C. The solution is stirred for about six hours at 50° C. and for about 16 hours at 20° C., then poured into cold water. The precipitate is collected by filtration, rinsed with water and dissolved in dichloromethane. The solution is washed with water and saturated sodium chloride solution, then dried. Evaporation provides yellow solid which is recrystallized from a benzene-hexane mixture to give 5-methylsulfonylmethyl-2-nitro-3-phenylbenzofuran, m.p. 178°-181° C.

Aufarbeitung

  1. additionA mixture of 2.8 g
  2. customrises to 50° C
  3. filtrationThe precipitate is collected by filtration
  4. washrinsed with water
  5. dissolutiondissolved in dichloromethane
  6. washThe solution is washed with water and saturated sodium chloride solution
  7. customdried
  8. customEvaporation
  9. customprovides yellow solid which
  10. customis recrystallized from a benzene-hexane mixture

Quellen und Nachweise

ORD-Eintrag
ord-bb0961efe26544cd9bc0c4ca2633e311
Quelldatensatz
uspto-grants-1979_05
Patentnummer
US04153716

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