HRID9342

反应详情

EQUATION

反应方程式

HRID 9342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In an evaporated schlenk flask kept under nitrogen atmosphere were added {4-[3,3-bis-(4-bromo-phenyl)-allylsulfanyl]-2-methyl-phenoxy}-acetic acid (231 mg, 0.42 mmol, example 1, step A–B), 3-(trifluoromethyl)phenylboronic acid (203 mg, 1.1 mmol), KF (81 mg, 1.39 mmol), Pd2(dba)3 (23 mg, 25 mmol) and Pd(P(t-Bu)3)2 (26 mg, 51 mmol). THF (5 ml) was added to the solid mixture keeping the mixture under nitrogen. The reaction mixture was stirred at room temperature for 1 h, followed by 10 h at 50° C. A saturated solution of ammonium chloride (5 ml) was added, and the mixture was extracted with dichloromethane (2×20 ml). The organic phases were dried and evaporated. The residue was purified by HPLC to give the title compound in 140 mg (49%) yield.

WORKUP

后处理

  1. customIn an evaporated schlenk flask kept under nitrogen atmosphere
  2. waitfollowed by 10 h at 50° C
  3. extractionthe mixture was extracted with dichloromethane (2×20 ml)
  4. customThe organic phases were dried
  5. customevaporated
  6. customThe residue was purified by HPLC