HRID1440491

反应详情

EQUATION

反应方程式

HRID 1440491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 500 ml of carbon tetrachloride, 50.5 g of the (2S,5S)-5-bromo-2-tert-butyl-5-methyl-1,3-dioxolan-4-one obtained in Step 2 was dissolved. To the resulting solution, 50.0 g of triethylamine was added, and the solution was refluxed for 4 hours. After the reaction solution was left to have cooled, insolubles were separated by filtration, the carbon tetrachloride was evaporated under reduced pressure, and the resulting residue was recrystallized from hexane to obtain 29.5 g of (2S)-2-tert-butyl-5-methylene-1,3-dioxolan-4-one.

WORKUP

后处理

  1. temperaturethe solution was refluxed for 4 hours
  2. waitAfter the reaction solution was left
  3. temperatureto have cooled
  4. custominsolubles were separated by filtration
  5. customthe carbon tetrachloride was evaporated under reduced pressure
  6. customthe resulting residue was recrystallized from hexane