تفاعل #2139924

ord-e3e4ddff55fb4d9fbf83ffd6880dc13d

معادلة التفاعل

O=C1C=CC=C2C1=Cc1ccccc12
fluorenone
Brc1ccccc1-c1ccccc1
2-bromobiphenyl
c1ccc2c(c1)-c1ccccc1C21c2ccccc2-c2ccccc21
9.9′-Spirobifluorene
المردود 80.0%

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    درجة الحرارةrefluxed
  3. 3
    ترشيحThe produced yellow precipitate was filtered
  4. 4
    workup.STIRRINGstirred in cold ammonium chloride
  5. 5
    ترشيحthe obtained crystal was filtered again
  6. 6
    أخرىdried
  7. 7
    workup.ADDITIONThereafter, acetic acid was added to the solid product
  8. 8
    درجة الحرارةthe solution was refluxed
  9. 9
    workup.STIRRINGwhile stirring
  10. 10
    workup.ADDITIONA small amount of hydrochloric acid was added
  11. 11
    أخرىto obtain the solid target compound
  12. 12
    ترشيحThe solid target compound was filtered
  13. 13
    غسيلwashed
  14. 14
    أخرىto obtain pure target compound with the yield of 80%

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07326474B2uspto-grants-2008_02