تفاعل #360938
ord-ccbe35180d5349e08245fb39f2fbce2d
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةAfter heating with a water bath for 3.5 hours
- 2درجة الحرارةthe mixture was cooled with ice
- 3ترشيحfiltered
- 4workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure
- 5workup.DISSOLUTIONThe residue was dissolved in ethanol
- 6ترشيحThe solution was filtrated
- 7أخرىto remove the insoluble matter
- 8workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure
- 9أخرىThe residue was recrystallized from water-
- 10workup.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).