HRID704136

反应详情

EQUATION

反应方程式

HRID 704136 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-t-butyl-3-iodomethyl-(1,5-dioxaspiro[5,5]undecane) (3.5 g.), p-toluenesulphonic acid (0.5 g.) and acetone (200 ml.) was refluxed for 36 hours. The mixture was cooled and sodium hydrogen carbonate (2.0 g.) was added. The solvent was removed in vacuo and the resulting oil was poured into water. The aqueous mixture was extracted with diethyl ether. The ethereal extracts were washed with water, dried over anhydrous magnesium sulphate and then evaporated in vacuo. 5-t-Butyl-2,2-dimethyl-5-iodomethyl-1,3-dioxane was obtained as a colourless oil (2.3 g.) and was used without further purification.

WORKUP

后处理

  1. temperaturewas refluxed for 36 hours
  2. temperatureThe mixture was cooled
  3. customThe solvent was removed in vacuo
  4. additionthe resulting oil was poured into water
  5. extractionThe aqueous mixture was extracted with diethyl ether
  6. washThe ethereal extracts were washed with water
  7. dry with materialdried over anhydrous magnesium sulphate
  8. customevaporated in vacuo