Hydrazine hydrate (1:1) → HCID 23332954, Verbindung

HRID 224404Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 224404
[Cl:1][C:2]([Cl:23])([Cl:22])[CH:3]1[O:8][CH:7]([C:9](Cl)([Cl:11])[Cl:10])[C:6]2[CH:13]=[C:14]([C:17](OCC)=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1.O.[NH2:25][NH2:26]>C(O)C>[Cl:10][C:9]([Cl:11])=[C:7]1[C:6]2[CH:13]=[C:14]([C:17]([NH:25][NH2:26])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4][CH:3]([C:2]([Cl:23])([Cl:22])[Cl:1])[O:8]1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 23332965HCID 23332965, Verbindung

Produkt 1

HCID 23332954HCID 23332954, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of ethyl 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylate (6.4 g.), 100% hydrazine hydrate (3 ml.) and ethanol (30 ml.) was warmed on the steam bath for 30 hours. The reaction mixture was cooled, and then evaporated to dryness under reduced pressure. The oily residue was triturated with petroleum ether (b.p. 60°-80° C.) and the solid product thus obtained was crystallised from ethanol, to give 4-dichloromethylene-2-trichloromethylbenzo[1,3]dioxin-6-carbohydrazide, m.p. 182°-183° C.

Aufarbeitung

  1. temperaturewas warmed on the steam bath for 30 hours
  2. temperatureThe reaction mixture was cooled
  3. customevaporated to dryness under reduced pressure
  4. customThe oily residue was triturated with petroleum ether (b.p. 60°-80° C.)
  5. customthe solid product thus obtained
  6. customwas crystallised from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-4583f278911a4bb1873c82e43ddf6246
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04232032

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