반응 #4210

ord-c98143d1d5664d11907a5d25e56ab78d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타rose to 40° C.
  2. 2
    workup.DISSOLUTIONthe starting material completely dissolved
  3. 3
    기타yielding a clear, colorless solution which
  4. 4
    workup.WAITAfter standing for one hour
  5. 5
    여과the crystallized product was filtered
  6. 6
    세척washed with cold water (200 ml)
  7. 7
    기타dried in vacuo overnight at room temperature

실험 절차

A suspension of α-chloro-3',4'-dihydroxyacetophenone (9.33 g, 0.05 mole) in 78 ml of acetic anhydride was treated with 0.1 ml of concentrated sulfuric acid and stirred for 1.5 hours under an argon atmosphere. Initially, the reaction temperature rose to 40° C. and the starting material completely dissolved yielding a clear, colorless solution which was poured onto approximately 300 g of crushed ice. After standing for one hour, the crystallized product was filtered, washed with cold water (200 ml) and dried in vacuo overnight at room temperature; yield: 11.5 g.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04723002uspto-grants-1988_02