HRID1423951

反应详情

EQUATION

反应方程式

HRID 1423951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

[(8-Bromo-6-chloro-4-hydroxy-2-oxo-2H-thiochromene-3-carbonyl)-amino]-acetic acid ethyl ester (22(d)) (500 mg, 1.2 mmol) was dissolved in anhydrous DMF (5 mL). To the solution was added Tributyl-phenyl-stannane (467 uL, 1.43 mmol), bis(triphenylphosphino) palladium(II) dichloride (100 mg, 0.12 mmol) and 4 A molecular sieves. The reaction was sealed and the solution was heated to 120 C for 45 minutes. The reaction was cooled, diluted with ethyl acetate (25 mL) and water (25 mL). The organic phase was separated, dried over magnesium sulfate and concentrated residue in vacuo. The residue was filtered through silica to provide the title compound (418 mg) which was used directly without further purification.

WORKUP

后处理

  1. customThe reaction was sealed
  2. temperaturethe solution was heated to 120 C for 45 minutes
  3. temperatureThe reaction was cooled
  4. customThe organic phase was separated
  5. dry with materialdried over magnesium sulfate and concentrated residue in vacuo
  6. filtrationThe residue was filtered through silica