HRID653678

反应详情

EQUATION

反应方程式

HRID 653678 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

81.9 g of 4-(dioxolan-2-yl)-3,3-dimethylbutanol, prepared above, are dissolved in 600 ml of chloroform, stabilized with amylene, in the presence of 62 ml of triethylamine. The mixture is cooled to 5° C. and 81 ml of mesyl chloride are added dropwise. The mixture is subsequently stirred for 4 hours at 5° C. and then left overnight at this temperature, washed with cold water and evaporated at 30° C. under vacuum. The residue obtained is taken up with ether and washed with sodium bicarbonate. The ether phase is dried over magnesium sulfate and then evaporated at 30° C. under vacuum to give 93.5 g of 4-(dioxolan-2-yl)-3,3-dimethylbutanol mesylate.

WORKUP

后处理

  1. waitleft overnight at this temperature
  2. washwashed with cold water
  3. customevaporated at 30° C. under vacuum
  4. customThe residue obtained
  5. washwashed with sodium bicarbonate
  6. dry with materialThe ether phase is dried over magnesium sulfate
  7. customevaporated at 30° C. under vacuum