반응 #170955

ord-9345771dbcee4f08a6d77263cf5b208c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 16 hours
  2. 2
    workup.DISTILLATIONAcetone was distilled
  3. 3
    workup.ADDITIONwater (5 L) was added
  4. 4
    여과Crude 1 was filtered
  5. 5
    기타dried
  6. 6
    기타recrystallised from a mixture of toluene:hexane (1:5)

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846845B2uspto-grants-2014_09