HRID2038387

反应详情

EQUATION

反应方程式

HRID 2038387 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

At room temperature, 7.2 ml of an aqueous 2M sodium carbonate solution and 167 mg (0.144 mmol) of tetrakis(triphenylphosphine)palladium are added to 1.00 g (2.89 mmol) of the compound from Example 5A and 714 mg (4.33 mmol) of the boronic acid from Example 22A in 40 ml of DME, and the mixture is subsequently stirred at 80° C. for 24 h. A saturated aqueous ammonium chloride solution is added, and the reaction mixture is subsequently extracted with dichloromethane. The organic phase is dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue is purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient). 606 mg (53% of theory) of the title compound having a purity of 90% are obtained.

WORKUP

后处理

  1. extractionthe reaction mixture is subsequently extracted with dichloromethane
  2. dry with materialThe organic phase is dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient)
  6. customare obtained