反応 #1563874

ord-12cb41b9b5e545edb357693a708b51fc

反応方程式

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)

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度under reflux for 30 minutes
  3. 3
    温度The reaction mixture was then cooled in an ice bath
  4. 4
    その他A solid precipitated
  5. 5
    ろ過the precipitate was collected by filtration
  6. 6
    洗浄washed with hexane

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09402397B2uspto-grants-2016_08