تفاعل #360938

ord-ccbe35180d5349e08245fb39f2fbce2d

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter heating with a water bath for 3.5 hours
  2. 2
    درجة الحرارةthe mixture was cooled with ice
  3. 3
    ترشيحfiltered
  4. 4
    workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in ethanol
  6. 6
    ترشيحThe solution was filtrated
  7. 7
    أخرىto remove the insoluble matter
  8. 8
    workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure
  9. 9
    أخرىThe residue was recrystallized from water-
  10. 10
    workup.ADDITIONcontaining methanol

الإجراء التجريبي

70 ml of ethanol and 15 ml of carbon disulfide were added to 2.6 g of 3,4-diaminoanisole and then a solution of 1.5 g of sodium hydroxide in 5 ml of water was added thereto. After heating with a water bath for 3.5 hours, the mixture was cooled with ice, filtered and then the solvent in the filtrate was distilled off under reduced pressure. The residue was dissolved in ethanol. The solution was filtrated to remove the insoluble matter and then the solvent in the filtrate was distilled off under reduced pressure. The residue was recrystallized from water-containing methanol to obtain 2.0 g of the titled compound (13).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05387600uspto-grants-1995_02