تفاعل #6455

ord-b0cbbbccef144c919960c98519e95613

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGWhile stirring under ice cooling
  2. 2
    درجة الحرارةby heating at 80° C. for further an hour
  3. 3
    workup.STIRRINGwith stirring
  4. 4
    أخرىAfter completion of the reaction
  5. 5
    ترشيحThe crystals were filtered
  6. 6
    غسيلwashed with water
  7. 7
    أخرىdried

الإجراء التجريبي

With stirring at 0° C., 8.06 g (50.0 mmols) of 5-methylisatin was added by small portions to a solution of 2.00 g (50.0 mmols) of sodium hydride in toluene. While stirring under ice cooling, 4.7 ml (50.0 mmols) of acetic anhydride was dropwise added to the mixture followed by heating at 80° C. for further an hour with stirring. After completion of the reaction, an aqueous saturated sodium bicarbonate solution was added to the reaction mixture. The crystals were filtered, washed with water and dried to give 4.84 g (yield, 47%) of 1-acetyl-5-methylisatin.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05248684uspto-grants-1993_09