Trifluoroacetic acid → HCID 23271750、化合物

HRID 550331ノート

反応式

HRID 550331 の反応式
[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

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 23150364HCID 23150364、化合物

生成物 1

HCID 23271750HCID 23271750、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a4969e7452bf4b34b31f6858f721d6e8
出典データセット
uspto-grants-2011_05
特許番号
US07947382B2

反応ノート

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