반응 #615770

반응 방정식

1-bromo-4-iodo-2-methoxybenzene

3-fluorophenylboronic acid

potassium phosphate

water

→

4-Bromo-3′-Fluoro-3-Methoxy-1,1′-Biphenyl

용매

DCM

dioxane

반응 조건

후처리

1. 1
   기타separated from the aqueous via phase separator (Radleys Discovery Technologies)
2. 2
   농축After concentration in vacuo
3. 3
   기타the material was purified via MPLC (12-g Redi Sep Gold)
4. 4
   세척eluting with 0-100% ethyl acetate in heptanes
5. 5
   기타to yield
6. 6
   농축after concentration, 4-bromo-3′-fluoro-3-methoxy-1,1′-biphenyl as an orange oil, which
7. 7
   기타was used without further purification

실험 절차

A solution of PdCl2(dppf)-CH2Cl2 adduct (0.065 g, 0.080 mmol), 1-bromo-4-iodo-2-methoxybenzene (CombiBlocks, 0.250 g, 0.799 mmol), 3-fluorophenylboronic acid (0.123 g, 0.879 mmol) and potassium phosphate (0.848 g, 3.99 mmol) in dioxane (2.130 ml)/water (1.065 ml) was heated to 90° C. overnight. The reaction was diluted with DCM and separated from the aqueous via phase separator (Radleys Discovery Technologies). After concentration in vacuo, the material was purified via MPLC (12-g Redi Sep Gold), eluting with 0-100% ethyl acetate in heptanes to yield, after concentration, 4-bromo-3′-fluoro-3-methoxy-1,1′-biphenyl as an orange oil, which was used without further purification.

출처