反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture is refluxed 1 hr
- temperature, cooled
- temperatureThe mixture is refluxed an additional 2 hrs
- temperature, cooled
- customThe layers are separated
- extractionthe aqueous layer is extracted with ether
- extractionextracted with chloroform
- extractionThe chloroform extract
- washis washed with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customthe solvent evaporated