HRID1533694

反应详情

EQUATION

反应方程式

HRID 1533694 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 43.79 g acetic acid 3-(4-tert-butyl-phenyl)-2-methyl-propenyl ester in 200 ml of THF was cooled to −70° C. A solution of 27.16 g potassium-tert-butoxide in 200 ml of THF was added at −70° C. during 20 min. and the resulting reaction mixture was stirred for 90 min. at the same temperature. Then a solution of 53.00 g 4-oxo-undecanoyl chloride in 200 ml of THF was dropped in and the reaction mixture was stirred for another 2.5 hours at −70° C. Then the reaction mixture was diluted with ether, washed with saturated NaHCO3 and brine. The organic phase was dried, filtered and evaporated to dryness. The residue was thin-layer distilled and purified by chromatography to yield 25.73 g of a yellow oil.

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. stirringwas stirred for another 2.5 hours at −70° C
  3. washwashed with saturated NaHCO3 and brine
  4. customThe organic phase was dried
  5. filtrationfiltered
  6. customevaporated to dryness
  7. distillationdistilled
  8. custompurified by chromatography