HRID1169174

反应详情

EQUATION

反应方程式

HRID 1169174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 43.79 g acetic acid 3-(4-tert-butyl-phenyl)-2-methyl-propenyl ester in 200 ml of tetrahydrofuran, a solution of 27.16 g potassium tert-butoxide in 200 ml of tetrahydrofuran was added at −78° C. After stirring at this temperature for 90 minutes, a solution of 53.00 g 4-oxo-undecanoyl chloride in 200 ml of tetrahydrofuran was added. After stirring at −78° C. for 2.5 hours, the solution was quenched with saturated sodium bicarbonate solution and diluted with ether. The organic phase was washed with saturated sodium bicarbonate solution and brine, dried and evaporated to dryness. The residue was purified by thin-film distillation and chromatography to yield 25.73 g of a yellow oil.

WORKUP

后处理

  1. stirringAfter stirring at −78° C. for 2.5 hours
  2. customthe solution was quenched with saturated sodium bicarbonate solution
  3. additiondiluted with ether
  4. washThe organic phase was washed with saturated sodium bicarbonate solution and brine
  5. customdried
  6. customevaporated to dryness
  7. distillationThe residue was purified by thin-film distillation and chromatography