反应 #1563874

ord-12cb41b9b5e545edb357693a708b51fc

反应方程式

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)

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  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
    其他A solid precipitated
  5. 5
    过滤the precipitate was collected by filtration
  6. 6
    洗涤washed with hexane

实验过程

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.

来源

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