Ammonium Chloride → Ici 111075

HRID 224405Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 224405
[Cl:1][C:2]([Cl:21])([Cl:20])[CH:3]1[O:8][CH:7]([C:9](Cl)([Cl:11])[Cl:10])[C:6]2[CH:13]=[C:14]([C:17]([OH:19])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1.[Cl-].[NH4+].[N-]=[N+]=[N-].[Na+]>CS(C)=O>[Cl:11][C:9]([Cl:10])=[C:7]1[C:6]2[CH:13]=[C:14]([C:17]([OH:19])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4][CH:3]([C:2]([Cl:1])([Cl:21])[Cl:20])[O:8]1

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 1941342,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxine-6-carboxylic acid

Produkt 1

HCID 194133Ici 111075

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

A mixture of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylic acid (2.08 g.), ammonium chloride (0.33 g.) and sodium azide (0.36 g.) in anhydrous dimethylsulphoxide (10 ml.) was warmed on the steam bath for 16 hours. The reaction mixture was cooled, poured onto ice and kept for 16 hours. The white product was filtered off, washed with water and dried, and crystallised from aqueous ethanol to give 4-dichloromethylene-2-trichloromethybenzo[1,3]dioxin-6-carboxylic acid, m.p. 222°-223° C.

Aufarbeitung

  1. temperaturewas warmed on the steam bath for 16 hours
  2. temperatureThe reaction mixture was cooled
  3. additionpoured onto ice
  4. filtrationThe white product was filtered off
  5. washwashed with water
  6. customdried
  7. customcrystallised from aqueous ethanol

Quellen und Nachweise

ORD-Eintrag
ord-20721285dce144de865526e89ff4f2a1
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04232032

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