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HCID 19744879, 화합물 → 1-Propanone, 1-(2,4-dihydroxyphenyl)-3-(3,4-dihydroxyphenyl)-

HRID 1030754
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HRID 1030754 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 19744879HCID 19744879, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 21893726Hydrochloride methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-653aa007b71546cb8c339c907225aea9
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05106871

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