تفاعل #72075

ord-9fd42774e03b4419938ca01fdb1efa66

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe reaction solution was concentrated under reduced pressure
  2. 2
    workup.ADDITIONdiluted with ethyl acetate
  3. 3
    غسيلwashed with water
  4. 4
    تجفيفdried over anhydrous sodium sulfate
  5. 5
    تركيزconcentration under reduced pressure
  6. 6
    أخرىthe residue was recrystallized from ethyl acetate/hexane

الإجراء التجريبي

2,4-Dinitrobenzonitrile (5.08 g, 26.3 mmol) was dissolved in DMF (55 ml). Potassium carbonate (4.36 g, 31.6 mmol) and ethyl thioglycolate (3.17 g, 26.3 mmol) were added, and the mixture was stirred at room temperature for three days. The reaction solution was concentrated under reduced pressure, diluted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was recrystallized from ethyl acetate/hexane to obtain 2.27 g of the title compound as crystals (32%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536197B2uspto-grants-2013_09