HRID704131

反应详情

EQUATION

反应方程式

HRID 704131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

and (iii) 5-Acetylthiomethyl-5-ethyl-2,2-dimethyl-1,3-dioxane (2.0 g.) was stirred at 20°, in 10% aqueous sodium hydroxide solution (2.0 ml.) in methanol (20 ml.), for 24 hours under nitrogen. The mixture was neutralized with concentrated hydrochloric acid (0.5 ml.). Dowex 50×8-200 ion exchange resin (H+ form) (1.0 g.) was added and the mixture was refluxed with stirring, under nitrogen, for 4 hours. The mixture was filtered and the filtrate was evaporated in vacuo. Toluene was added to the residue and the mixture was evaporated in vacuo. 2,2-Di-(hydroxymethyl)-butanethiol was obtained as a colourless oil and was used without further purification (1.0 g.)

WORKUP

后处理

  1. additionDowex 50×8-200 ion exchange resin (H+ form) (1.0 g.) was added
  2. temperaturethe mixture was refluxed
  3. filtrationThe mixture was filtered
  4. customthe filtrate was evaporated in vacuo
  5. additionToluene was added to the residue
  6. customthe mixture was evaporated in vacuo