Reaktion #1563874

ord-12cb41b9b5e545edb357693a708b51fc

Reaktionsgleichung

O=C(c1cccs1)C1Oc2c(Cl)c(Cl)c(Cl)c(Cl)c2O1
(4,5,6,7-tetrachlorobenzo[d][1,3]dioxol-2-yl)(thiophen-2-yl)methanone
NNc1ccccc1
phenyl hydrazine
C(=NNc1ccccc1)C(=NNc1ccccc1)c1cccs1
2,2′-(1-(thiophen-2-yl)ethane-1,2-diylidene)bis(1-phenylhydrazine)

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux for 30 minutes
  3. 3
    TemperaturThe reaction mixture was then cooled in an ice bath
  4. 4
    SonstigeA solid precipitated
  5. 5
    Filtrationthe precipitate was collected by filtration
  6. 6
    Waschenwashed with hexane

Vorschrift

A mixture of (4,5,6,7-tetrachlorobenzo[d][1,3]dioxol-2-yl)(thiophen-2-yl)methanone (1 g, 2.70 mmol) and phenyl hydrazine (880 mg, 8.13 mmol) in ethanol (14 mL) was heated under reflux for 30 minutes. The reaction mixture was then cooled in an ice bath. A solid precipitated, and the precipitate was collected by filtration and washed with hexane. Crude 2,2′-(1-(thiophen-2-yl)ethane-1,2-diylidene)bis(1-phenylhydrazine) was obtained as a brown solid (500 mg, 57.8% yield) and used in the next step without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09402397B2uspto-grants-2016_08