تفاعل #792197

ord-0516f1e417c84e7fa01b74f129b935bf

معادلة التفاعل

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)

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةunder reflux for 30 minutes
  3. 3
    درجة الحرارةThe reaction mixture was then cooled in an ice bath
  4. 4
    أخرىA solid precipitated
  5. 5
    ترشيحthe precipitate was collected by filtration
  6. 6
    غسيلwashed with hexane

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09173401B2uspto-grants-2015_11