تفاعل #170955

ord-9345771dbcee4f08a6d77263cf5b208c

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةrefluxed for 16 hours
  2. 2
    workup.DISTILLATIONAcetone was distilled
  3. 3
    workup.ADDITIONwater (5 L) was added
  4. 4
    ترشيحCrude 1 was filtered
  5. 5
    أخرىdried
  6. 6
    أخرىrecrystallised from a mixture of toluene:hexane (1:5)

الإجراء التجريبي

Ethyl bromoacetate (452 g, 2.7 mol.) was added to a mixture of paracetamol (300 g, 1.984 mol) and anhydrous K2CO3 (1.80 kg, 7.814 mmol) in anhydrous acetone (3 L) and refluxed for 16 hours. Acetone was distilled and water (5 L) was added. Crude 1 was filtered, dried and recrystallised from a mixture of toluene:hexane (1:5) to give pure 1 (377 grams, 80%) as a white shining powder. The melting point was found to be 104.2-106.2° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08846845B2uspto-grants-2014_09