HRID1605816

反应详情

EQUATION

反应方程式

HRID 1605816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a well stirred solution of 1.2 gm. (0.01 mole) of allyl bromide in 50 ml. of benzene, a solution of 1.5 gm. (0.01 mole) of 4-azatricyclo[4.3.1.13,8 ]undecane in 50 ml. of benzene is added dropwise. The mixture is refluxed 1 hr., cooled, and 1 gm. of acetic anhydride is added. The mixture is refluxed an additional 2 hrs., cooled, poured into ice water and acidified with acetic acid. The layers are separated and the aqueous layer is extracted with ether. The acidic aqueous layer is made basic with NaOH, and extracted with chloroform. The chloroform extract is washed with water, dried over magnesium sulfate, filtered and the solvent evaporated to give 4-allyl- 4-azatricyclo[4.3.1.13,8 ]undecane.

WORKUP

后处理

  1. temperatureThe mixture is refluxed 1 hr
  2. temperature, cooled
  3. temperatureThe mixture is refluxed an additional 2 hrs
  4. temperature, cooled
  5. customThe layers are separated
  6. extractionthe aqueous layer is extracted with ether
  7. extractionextracted with chloroform
  8. extractionThe chloroform extract
  9. washis washed with water
  10. dry with materialdried over magnesium sulfate
  11. filtrationfiltered
  12. customthe solvent evaporated