HRID1387282

反应详情

EQUATION

反应方程式

HRID 1387282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of bis(triphenylphosphine)Pd(II) chloride (0.014 g), lithium chloride (0.067 g), 1-hexyl-5-iodo-4-methyl-3-nitro-2-pyridone (0.15 g, 0.41 mmol) and phenyltributyltin (0.11 mL, 0.62 mmol) in THF (15 mL) was heated under reflux for 2 days. The mixture was cooled, diluted with ethyl acetate, and washed with aqueous potassium fluoride and water. The organic phase was dried, filtered and evaporated. Chromatography of the residue over silica gel (petroleum ether/methylene chloride 1/1 to methylene chloride is gradient) gave 1-hexyl-4-methyl-3-nitro-5-phenyl-2-pyridone (0.093 g, 72%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 days
  3. temperatureThe mixture was cooled
  4. washwashed with aqueous potassium fluoride and water
  5. customThe organic phase was dried
  6. filtrationfiltered
  7. customevaporated