반응 #42759

ord-7b4b11184e3f449b88142c800caa6db1

반응 방정식

CC(=O)c1ccc(O)cc1O
2′,4′-Dihydroxyacetophenone
COc1ccc(CCl)cc1
4-methoxybenzyl chloride
O=C([O-])[O-].[K+].[K+]
potassium carbonate
[I-].[K+]
potassium iodide
COc1ccc(COc2ccc(C(C)=O)c(O)c2)cc1
1-[2-Hydroxy-4-(4-methoxy-benzyloxy)-phenyl]ethanone

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ethyl acetate (3×100 ml)
  2. 2
    세척washed with saturated brine (100 ml)
  3. 3
    건조dried (MgSO4)
  4. 4
    여과filtered
  5. 5
    농축concentrated, until crystallization commences
  6. 6
    여과the crystals are recovered by filtration
  7. 7
    세척washed with cold ethyl acetate
  8. 8
    건조with n-hexane and dried

실험 절차

2′,4′-Dihydroxyacetophenone (11.71 g, 0.077 mol), 4-methoxybenzyl chloride (10.44 ml, 0.077 mol), anhydrous potassium carbonate (11.75 g, 0.085 mol) and potassium iodide (12.78 g, 0.077 mol) are heated together in refluxing dry acetone (80 ml) for 4 hours. The mixture is then cooled to room temperature, poured into water (250 ml) and extracted with ethyl acetate (3×100 ml). The ethyl acetate extracts are combined, washed with saturated brine (100 ml), dried (MgSO4), filtered and concentrated, until crystallization commences. After standing at 4° C. for 16 h, the crystals are recovered by filtration, washed with cold ethyl acetate and then with n-hexane and dried.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732435B2uspto-grants-2010_06