반응 #595079

반응 방정식

K2CO3

4-bromo-2-fluoro-1-iodobenzene

6

2-(2,3-Difluoro-4-trimethylsilylphenyl)-5,5-dimethyl-1,3,2-dioxaborinane

→

(4′-Bromo-2,3,2′-trifluorobiphenyl-4-yl)trimethylsilane

수율 88.0%

용매

water

dioxane

반응 조건

후처리

1. 1
   온도the mixture is refluxed overnight
2. 2
   세척The organic phase is washed with water and sat. NaCl
3. 3
   건조dried over MgSO4
4. 4
   여과filtered through SiO2
5. 5
   기타The solvent is removed under reduced pressure, petroleum ether
6. 6
   workup.ADDITIONis added to the oily residue
7. 7
   기타the product is recrystallised at −25° C. (yield: 88%, m.p. 78.0° C.)

실험 절차

A solution of 16.6 g (120 mmol) of K2CO3 in 50 ml of water is added to a solution of 15 g (50 mmol) of 4-bromo-2-fluoro-1-iodobenzene, 14.9 g (50 mmol) of 6 and 2.31 g (2 mmol) of [Pd(PPh3)4] in 100 ml of dioxane, and the mixture is refluxed overnight. The organic phase is washed with water and sat. NaCl, dried over MgSO4 and filtered through SiO2. The solvent is removed under reduced pressure, petroleum ether is added to the oily residue, and the product is recrystallised at −25° C. (yield: 88%, m.p. 78.0° C.).

출처