Potassium Iodide → 1-(2-Hydroxy-4-((4-methoxyphenyl)methoxy)phenyl)ethanone

HRID 14481

반응식

HRID 14481 반응식
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[C:9](=[O:11])[CH3:10].[CH3:12][O:13][C:14]1[CH:21]=[CH:20][C:17]([CH2:18]Cl)=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>O.CC(C)=O>[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH2:18][C:17]2[CH:20]=[CH:21][C:14]([O:13][CH3:12])=[CH:15][CH:16]=2)[CH:5]=[CH:4][C:3]=1[C:9](=[O:11])[CH3:10]

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 69902',4'-DihydroxyacetophenoneHCID 11430Potassium CarbonateHCID 699934-Methyloxybenzyl chloride

생성물 1

HCID 113232321-(2-Hydroxy-4-((4-methoxyphenyl)methoxy)phenyl)ethanone

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

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.

후처리

  1. extractionextracted with ethyl acetate (3×100 ml)
  2. washwashed with saturated brine (100 ml)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated, until crystallization commences
  6. filtrationthe crystals are recovered by filtration
  7. washwashed with cold ethyl acetate
  8. dry with materialwith n-hexane and dried

출처 및 근거

ORD 기록
ord-7b4b11184e3f449b88142c800caa6db1
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732435B2

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