反応 #2139924

反応方程式

fluorenone

2-bromobiphenyl

→

9.9′-Spirobifluorene

収率 80.0%

溶媒

ether

ether

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   温度refluxed
3. 3
   ろ過The produced yellow precipitate was filtered
4. 4
   workup.STIRRINGstirred in cold ammonium chloride
5. 5
   ろ過the obtained crystal was filtered again
6. 6
   その他dried
7. 7
   workup.ADDITIONThereafter, acetic acid was added to the solid product
8. 8
   温度the solution was refluxed
9. 9
   workup.STIRRINGwhile stirring
10. 10
    workup.ADDITIONA small amount of hydrochloric acid was added
11. 11
    その他to obtain the solid target compound
12. 12
    ろ過The solid target compound was filtered
13. 13
    洗浄washed
14. 14
    その他to obtain pure target compound with the yield of 80%

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%.

出典