Реакция #2139924

ord-e3e4ddff55fb4d9fbf83ffd6880dc13d

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added
  2. 2
    Температураrefluxed
  3. 3
    ФильтрацияThe produced yellow precipitate was filtered
  4. 4
    workup.STIRRINGstirred in cold ammonium chloride
  5. 5
    Фильтрацияthe obtained crystal was filtered again
  6. 6
    Другоеdried
  7. 7
    workup.ADDITIONThereafter, acetic acid was added to the solid product
  8. 8
    Температураthe solution was refluxed
  9. 9
    workup.STIRRINGwhile stirring
  10. 10
    workup.ADDITIONA small amount of hydrochloric acid was added
  11. 11
    Другоеto obtain the solid target compound
  12. 12
    ФильтрацияThe solid target compound was filtered
  13. 13
    Промывкаwashed
  14. 14
    Другоеto obtain pure target compound with the yield of 80%

Методика

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%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07326474B2uspto-grants-2008_02