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4-Ethoxy-3,3'-difluoro-4'-propyl-[1,1'-biphenyl]-2,2'-dicarboaldehyde → 2-Ethoxy-1,8-difluoro-7-propyl-9,10-dihydrophenanthrene-9,10-diol

HRID 718486
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HRID 718486 반응식
[CH2:1]([O:3][C:4]1[C:5]([F:24])=[C:6]([CH:22]=[O:23])[C:7]([C:10]2[C:11]([CH:20]=[O:21])=[C:12]([F:19])[C:13]([CH2:16][CH2:17][CH3:18])=[CH:14][CH:15]=2)=[CH:8][CH:9]=1)[CH3:2]>[Zn].[Cl-].[Zn+2].[Cl-].CN(C=O)C>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]2[C:10]3[C:11](=[C:12]([F:19])[C:13]([CH2:16][CH2:17][CH3:18])=[CH:14][CH:15]=3)[CH:20]([OH:21])[CH:22]([OH:23])[C:6]=2[C:5]=1[F:24])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 866960644-Ethoxy-3,3'-difluoro-4'-propyl-[1,1'-biphenyl]-2,2'-dicarboaldehyde

생성물 1

HCID 680105352-Ethoxy-1,8-difluoro-7-propyl-9,10-dihydrophenanthrene-9,10-diol수율 59.7%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 3007855Zincchloride촉매HCID 6228Dimethylformamide용매

실험 절차

Under a nitrogen atmosphere, zinc powder (0.295 g, 4.513 mmol) and zinc chloride (0.1 g, 0.752 mmol) were added to a DMF (5 mL) solution of compound (56) (0.5 g, 1.504 mmol), and the resultant mixture was agitated at 80° C. for 8 hours. The reaction mixture was quenched with 20 mL of 1N hydrochloric acid aqueous solution, and extracted with 10 mL of toluene three times. Combined organic layers were washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine, and then dried over magnesium sulfate, and a solvent was distilled off by an evaporator. The residue was purified by silica gel column chromatography, and thus 2-ethoxy-1,8-difluoro-7-propyl-9,10-dihydrophenanthrene-9,10-diol (57) (0.3 g, yield 59.7%) was obtained.

후처리

  1. customThe reaction mixture was quenched with 20 mL of 1N hydrochloric acid aqueous solution
  2. extractionextracted with 10 mL of toluene three times
  3. washCombined organic layers were washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine
  4. dry with materialdried over magnesium sulfate
  5. distillationa solvent was distilled off by an evaporator
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-1cc4e4ef27074eef8edce61201498f49
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09193908B2

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