HRID235707

反应详情

EQUATION

反应方程式

HRID 235707 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of about 3.75 g of lithium aluminum hydride in about 100 ml of ether at about 0° C., was added dropwise, under argon, over about 20 minutes, a solution of about 29 g of 2-methyl-α-octadecyl-1,3-dioxolan-2-propanoic acid, ethyl ester in about 200 ml of ether. This mixture was stirred about 40 minutes at room temperature, then about 15 ml of ethyl acetate were added dropwise, followed by about 1.5 ml of water, about 3 ml of about 15% sodium hydroxide and about 4 ml of water. The mixture was then filtered through celite and the solid washed with ether. The solvent was removed from the filtrate, giving an oil which crystallized on standing, giving about 24.1 g of the desired title compound, mp 34°-35° C.

WORKUP

后处理

  1. additionwas added dropwise, under argon, over about 20 minutes
  2. filtrationThe mixture was then filtered through celite
  3. washthe solid washed with ether
  4. customThe solvent was removed from the filtrate
  5. customgiving an oil which
  6. customcrystallized