HRID325932

反应详情

EQUATION

反应方程式

HRID 325932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Ten milliliters of benzene was added to 4.51 g of 5-butylpicolinic acid, and 9 g of thionyl chloride was further added. The mixture was heated under reflux for 22 minutes. The excess of thionyl chloride and benzene were disiled off under reduced pressure, and 10 ml of benzene was added to the residue. The mixture was cooled to 0° C. and stirred. To the solution was added dropwise a solution of 5 g of dl-α-tocopherol in 4.25 ml of pyridine to perform the reaction for 1 hour and 40 minutes. The insoluble matter was removed by filtration from the reaction mixture, and the residue was washed with water, 1 N hydrochloric acid, water, a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride in this order. Benzene was distilled off, and the residue was chromatographed on a silica gel column using benzene/ethyl acetate (4:1) as an eluent to give 3.2 g of dl-α-tocopheryl 5-butylpicolinate.

WORKUP

后处理

  1. additionwas further added
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 22 minutes
  4. additionwas added to the residue
  5. customthe reaction for 1 hour
  6. custom40 minutes
  7. customThe insoluble matter was removed by filtration from the reaction mixture
  8. washthe residue was washed with water, 1 N hydrochloric acid, water
  9. distillationBenzene was distilled off
  10. customthe residue was chromatographed on a silica gel column