HRID2352192

反应详情

EQUATION

反应方程式

HRID 2352192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

The reaction was carried out under nitrogen atmosphere in a three neck flask equipped with a magnetic stirring bar, reflux condenser, addition funnel and thermometer. 50 ml of 1-butanol and 667 mg (2.5 mmoles) of cadmium acetate dihydrate was introduced and the catalyst was dissolved by slight warming. 18.13 g (100 mmoles) of undecyl cyanide was added and the solution was heated to 125° C. 7.33 g (120 mmoles) of 2-aminoethanol was then added dropwise controlling the evolution of ammonia. At the end of the reaction (ca. 48 hrs.) the solvent was removed under vacuo. The residue was treated with 100 ml of petroleum ether and filtered after keeping for several hours. The filtrate was washed with water, dried over anhydrous magnesium sulfate, concentrated and the residue was distilled 114° C./0.5mm to give 19.83 g (88%) of 2-undecyl-2oxazoline.

WORKUP

后处理

  1. customequipped with a magnetic stirring bar
  2. temperaturereflux
  3. additioncondenser, addition funnel
  4. dissolutionthe catalyst was dissolved by slight warming
  5. customAt the end of the reaction (ca. 48 hrs.) the solvent
  6. customwas removed under vacuo
  7. additionThe residue was treated with 100 ml of petroleum ether
  8. filtrationfiltered
  9. waitafter keeping for several hours
  10. washThe filtrate was washed with water
  11. dry with materialdried over anhydrous magnesium sulfate
  12. concentrationconcentrated
  13. distillationthe residue was distilled 114° C./0.5mm