반응 #1563874

ord-12cb41b9b5e545edb357693a708b51fc

반응 방정식

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)

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도under reflux for 30 minutes
  3. 3
    온도The reaction mixture was then cooled in an ice bath
  4. 4
    기타A solid precipitated
  5. 5
    여과the precipitate was collected by filtration
  6. 6
    세척washed with hexane

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09402397B2uspto-grants-2016_08