HRID528588

反应详情

EQUATION

反应方程式

HRID 528588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customseparated from the aqueous via phase separator (Radleys Discovery Technologies)
  2. concentrationAfter concentration in vacuo
  3. customthe material was purified via MPLC (12-g Redi Sep Gold)
  4. washeluting with 0-100% ethyl acetate in heptanes
  5. customto yield
  6. concentrationafter concentration, 4-bromo-3′-fluoro-3-methoxy-1,1′-biphenyl as an orange oil, which
  7. customwas used without further purification