2,7-Dibromo-9-fluorenone → 9-(2-Biphenylyl)-2,7-dibromo-9-fluorenol

HRID 1499975ノート

反応式

HRID 1499975 の反応式
[Br:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([Br:15])=[CH:9][CH:10]=3)[C:5](=[O:16])[C:4]=2[CH:3]=1>C(OCC)C>[C:11]1([C:12]2[CH:4]=[CH:3][CH:2]=[CH:14][CH:13]=2)[CH:6]=[CH:7][CH:8]=[CH:9][C:10]=1[C:5]1([OH:16])[C:4]2[CH:3]=[C:2]([Br:1])[CH:14]=[CH:13][C:12]=2[C:11]2[C:6]1=[CH:7][C:8]([Br:15])=[CH:9][CH:10]=2

参加物

3

反応物 1

HCID 2599222,7-Dibromo-9-fluorenone

生成物 1

HCID 220160479-(2-Biphenylyl)-2,7-dibromo-9-fluorenol収率 198.7%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
50 °C

実験手順

15.2 g (45 mmol) of 2,7-dibromo-9-fluorenone was put in a 100 mL three-necked flask, and nitrogen substitution was conducted. 40 mL of diethyl ether was added. The Grignard reagent above was transferred into a dropping funnel by a cannula so as not to expose it to the atmosphere, and was added dropwise into the mixture. The mixture was refluxed at 50° C. After the reaction, the solution was washed with water. Then the aqueous layer was extracted with ethyl acetate and combined with the organic layer. The layers were washed with a saturated saline solution, then dried with magnesium sulfate. Filtration and concentration were carried out, and 22 g of 9-(biphenyl-2-yl)-2,7-dibromo-9-fluorenol was obtained as a white solid, in a yield of 90%.

後処理

  1. additionwas added dropwise into the mixture
  2. customAfter the reaction
  3. washthe solution was washed with water
  4. extractionThen the aqueous layer was extracted with ethyl acetate
  5. washThe layers were washed with a saturated saline solution
  6. dry with materialdried with magnesium sulfate
  7. filtrationFiltration and concentration

出典と根拠

ORDレコード
ord-9c68108dc01e4e8495e2315128b22b47
出典データセット
uspto-grants-2015_12
特許番号
US09203035B2

反応ノート

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