HRID255962

反应详情

EQUATION

反应方程式

HRID 255962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 80 g of (hexadecyloxy) acetic acid in 350 ml of tetrahydrofuran was stirred at 0° C. while 798.71 ml of 1M borane in tetrahydrofuran was added dropwise over one hour. When addition was complete the mixture was stirred 2 hours than 50 ml of acetone was added followed by 60 ml of water dropwise. The tetrahydrofuran was allowed to evaporate overnight, then the residue was mixed with water and chloroform and heated to dissolve the solid. The organic layer was separated, dried and the solvent removed. The residue was recrystallized from cold methanol, giving 70.6 g of the desired compound as a white solid, mp 42°-44° C.

WORKUP

后处理

  1. additionwas added dropwise over one hour
  2. additionWhen addition
  3. additionwas added
  4. customto evaporate overnight
  5. additionthe residue was mixed with water and chloroform
  6. temperatureheated
  7. dissolutionto dissolve the solid
  8. customThe organic layer was separated
  9. customdried
  10. customthe solvent removed
  11. customThe residue was recrystallized from cold methanol