反応 #65096

反応方程式

4-bromo-1-n-octyloxybenzene

benzene

sodium carbonate

2,3-difluorophenyl boronic acid

→

4-n-octyloxy-2', 3'-difluorobiphenyl

溶媒

ether

ethanol

反応条件

後処理

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   その他the solution thus formed
3. 3
   温度was heated
4. 4
   温度to reflux for 5 hours
5. 5
   温度After the solution was cooled
6. 6
   抽出to extract the product
7. 7
   洗浄washed with water
8. 8
   その他dried
9. 9
   workup.DISTILLATIONThe solvent was distilled off under a reduced pressure
10. 10
    その他The residue thus obtained
11. 11
    その他was purified by a silica gel column chromatography

実験手順

To a mixture of 4.2 g of the 4-bromo-1-n-octyloxybenzene, 0.5 g of tetrakis(triphenylphosphine) palladium(0), 53 ml of benzene, and 53 ml of an aqueous sodium carbonate solution (2 mol/liter), 26 ml of ethanol containing 3.0 g of 2,3-difluorophenyl boronic acid synthesized by the same method as in [1] in Example 1 was added dropwise, and then the solution thus formed was heated to reflux for 5 hours. After the solution was cooled, it was added with 200 ml of an ether to extract the product, washed with water and dried. The solvent was distilled off under a reduced pressure. The residue thus obtained was purified by a silica gel column chromatography using a mixed solvents of n-hexane and diethyl ether (10:2) to obtain 2.8 g of 4-n-octyloxy-2', 3'-difluorobiphenyl.

出典