HRID1987776

反应详情

EQUATION

反应方程式

HRID 1987776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.39 g of 2,4,6,7-tetramethyl-5-nitrodihydrobenzofuran-2-aldehyde and 31 g of 2-methyl-2-butene were dissolved in 190 ml of t-butanol and a solution prepared by dissolving 7.77 g of sodium chlorite and 10.1 g of sodium dihydrogen phospahte dehydrate in 78 ml of water was added dropwise under ice cooling, followed by stirring at room temperature for 2 hours. After 2-methyl-2-butene and t-butanol were distilled off under reduced pressure, water was added and the reaction solution was extracted with ether. The solution was washed with saturated saline and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure and the residue was crystallized from ether-hexane to obtain 1.20 g of the objective product.

WORKUP

后处理

  1. customa solution prepared
  2. additionwas added dropwise under ice cooling
  3. distillationAfter 2-methyl-2-butene and t-butanol were distilled off under reduced pressure, water
  4. additionwas added
  5. extractionthe reaction solution was extracted with ether
  6. washThe solution was washed with saturated saline
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. customthe residue was crystallized from ether-hexane