HRID1950693

反应详情

EQUATION

反应方程式

HRID 1950693 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-Pentadecanol of Example 5 (180 g) and dichloromethane (2500 ml) were added to a 5-litre three-necked flask. The mixture was cooled to 0° C., and carbon tetrabromide (313.6 g) was added and stirred until it dissolved. Triphenylphosphine (351.4 g) was then added dropwise. The resulting mixture was allowed to warm to ambient temperature and left stirring for two days. The reaction mixture was then filtered, and the solvent removed on a rotary evaporator at 56° C. The resulting solid was re-dissolved in heptane and left stirring for two days. It was then filtered through celite under vacuum, and the heptane removed on a rotary evaporator at 78° C. to yield the title compound.

WORKUP

后处理

  1. dissolutiondissolved
  2. temperatureto warm to ambient temperature
  3. waitleft
  4. stirringstirring for two days
  5. filtrationThe reaction mixture was then filtered
  6. customthe solvent removed on a rotary evaporator at 56° C
  7. dissolutionThe resulting solid was re-dissolved in heptane
  8. waitleft
  9. stirringstirring for two days
  10. filtrationIt was then filtered through celite under vacuum
  11. customthe heptane removed on a rotary evaporator at 78° C.