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HCID 19744879、化合物 → 1-Propanone, 1-(2,4-dihydroxyphenyl)-3-(3,4-dihydroxyphenyl)-

HRID 2254269
ノート
印刷プレビュー

反応式

HRID 2254269 の反応式
COC[O:4][C:5]1[CH:10]=[C:9]([O:11]COC)[CH:8]=[CH:7][C:6]=1[C:15](=[O:32])[CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([O:24]COC)=[C:20]([O:28]COC)[CH:19]=1>Cl.CO>[OH:4][C:5]1[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:6]=1[C:15](=[O:32])[CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([OH:24])=[C:20]([OH:28])[CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 19744879HCID 19744879、化合物

生成物 1

HCID 115508261-Propanone, 1-(2,4-dihydroxyphenyl)-3-(3,4-dihydroxyphenyl)-収率 39%

試薬・触媒・溶媒 1

HCID 21893726Hydrochloride methanol溶媒

実験手順

Then, 4.94 g of 1-[2,4-bis(methoxymethoxy)phenyl]-3-[3,4-bis(methoxymethoxy)phenyl]-1-propanone was dissolved in 48 ml of a hydrochloric acid/methanol reagent, and the solution was refluxed for 8 minutes and the reaction liquid was poured into ice water and extracted with ethyl acetate two times. The organic layer was washed with water three times, shaken with a saturated aqueous solution of sodium chloride, dried with anhydrous sodium sulfate and filtered, and the solvent was removed from the filtrate by distillation. The obtained residue was subjected to the column chromatography (400 g of 230-400 mesh silica gel, n-hexane/ethyl acetate=3/2, 0.5 kg/cm2). Fractions of 50 ml were collected, and the 96th to 120th fractions were combined and the solvent was removed by distillation. The residue was recrystallized from n-hexane and chloroform to obtain 453.6 mg (yield=39.0%) of 1-(2,4-dihydroxyphenyl)-3-(3,4-dihydroxyphenyl)-1-propanone.

後処理

  1. temperaturethe solution was refluxed for 8 minutes
  2. customthe reaction liquid
  3. extractionextracted with ethyl acetate two times
  4. washThe organic layer was washed with water three times
  5. dry with materialdried with anhydrous sodium sulfate
  6. filtrationfiltered
  7. customthe solvent was removed from the filtrate by distillation
  8. customFractions of 50 ml were collected
  9. customthe solvent was removed by distillation
  10. customThe residue was recrystallized from n-hexane and chloroform

出典と根拠

ORDレコード
ord-8f840d01c9c846509a732b8961964fe5
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05234951

反応ノート

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