반응 #2139924

반응 방정식

fluorenone

2-bromobiphenyl

→

9.9′-Spirobifluorene

수율 80.0%

용매

ether

ether

반응 조건

후처리

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

실험 절차

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%.

출처