HRID409937

反应详情

EQUATION

反应方程式

HRID 409937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 1.5 g of 1-bromo-3-nitrobenzene (7.42 mmol), 1 g of 5-formyl-2-furanboronic acid (7.42 mmol), and 35 mL of a solution of saturated sodium carbonate (Na2CO3) in 0.2 M tetrahydrofuran was added 0.2 g of tetrakis triphenylphosphine palladium [Pd(PPh3)4] (0.2 mmol) at room temperature with stirring. After completion of the addition, the resulting mixture was heated for an additional 12 hrs, cooled to room temperature, and concentrated in vacuo. The concentrate was extracted with methylene chloride, and the organic layer thus formed was added, washed with saturated brine, dried over magnesium sulfate, and concentrated in a vacuum. Purification by silica gel column chromatography afforded the title compound.

WORKUP

后处理

  1. additionAfter completion of the addition
  2. temperaturethe resulting mixture was heated for an additional 12 hrs
  3. concentrationconcentrated in vacuo
  4. extractionThe concentrate was extracted with methylene chloride
  5. customthe organic layer thus formed
  6. additionwas added
  7. washwashed with saturated brine
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated in a vacuum
  10. customPurification by silica gel column chromatography