2-Bromobiphenyl → 9,9'-Spirobi(9H-fluorene)

HRID 2052742

反応式

HRID 2052742 の反応式
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[C:14]1(=O)[C:26]2[C:18]([C:19]3[C:24]([CH:25]=2)=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:17][CH:16]=[CH:15]1>CCOCC>[CH:7]1[C:2]2[C:25]3([C:26]4[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=4[C:19]4[C:24]3=[CH:23][CH:22]=[CH:21][CH:20]=4)[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:3]=2[CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 163292-BromobiphenylHCID 22281833Fluoreneone

生成物 1

HCID 1359759,9'-Spirobi(9H-fluorene)収率 80%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

As shown in the following reaction 1, 6.1 g of 2-bromobiphenyl and 0.585 g of dried Mg were dissolved with ether, and 4.2 g of fluorenone dissolved in ether was added thereto, and refluxed while stirring overnight. The produced yellow precipitate was filtered, and stirred in cold ammonium chloride, and then the obtained crystal was filtered again and dried. Thereafter, acetic acid was added to the solid product, and the solution was refluxed while stirring. A small amount of hydrochloric acid was added thereto to obtain the solid target compound. The solid target compound was filtered and washed to obtain pure target compound with the yield of 80%.

後処理

  1. additionwas added
  2. temperaturerefluxed
  3. filtrationThe produced yellow precipitate was filtered
  4. stirringstirred in cold ammonium chloride
  5. filtrationthe obtained crystal was filtered again
  6. customdried
  7. additionThereafter, acetic acid was added to the solid product
  8. temperaturethe solution was refluxed
  9. stirringwhile stirring
  10. additionA small amount of hydrochloric acid was added
  11. customto obtain the solid target compound
  12. filtrationThe solid target compound was filtered
  13. washwashed
  14. customto obtain pure target compound with the yield of 80%

出典と根拠

ORDレコード
ord-e3e4ddff55fb4d9fbf83ffd6880dc13d
出典データセット
uspto-grants-2008_02
特許番号
US07326474B2

関連ノート

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