Trifluoroacetic acid → HCID 23271750, 화합물

HRID 550331노트

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HRID 550331 반응식
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9]([Br:16])=[CH:10][CH:11]=3)[C:6]([OH:18])(C)[C:5](O)([CH3:19])[C:4]=2[CH:3]=1.F[C:22](F)(F)C(O)=O>C(O)(=O)C>[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9]([Br:16])=[CH:10][CH:11]=3)[C:6](=[O:18])[C:5]([CH3:19])([CH3:22])[C:4]=2[CH:3]=1

참가 물질

4

실험 절차

132.8 g (294 mmol) of 2,7-dibromo-9,10-dihydroxy-9,10-dimethyl-9,10-dihydrophenanthrene were suspended in 420 ml of acetic acid and 210 ml of trifluoroacetic acid under argon, and the mixture was stirred for 3 h under reflux. After the mixture had been stirred overnight at room temperature, it was filtered with suction, the residue was washed with water and methanol and dissolved in toluene, the solution was filtered through silica gel, and the solvent was removed, giving 89.9 g (80.4% of theory) of the product, which was used without further purification.

후처리

  1. temperatureunder reflux
  2. filtrationit was filtered with suction
  3. washthe residue was washed with water and methanol
  4. dissolutiondissolved in toluene
  5. filtrationthe solution was filtered through silica gel
  6. customthe solvent was removed
  7. customgiving 89.9 g (80.4% of theory) of the product, which
  8. customwas used without further purification

출처 및 근거

ORD 기록
ord-a4969e7452bf4b34b31f6858f721d6e8
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947382B2

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