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 2 liter three-neck flask equipped with a dropping funnel, a reflux condenser and a stirrer was added 25.5 g (1.05 mole) of metallic magnesium and it was dried sufficiently to supplying dry nitrogen gas. After that, 50 ml of tetrahydrofuran which has been dried with a molecular sieve 5A, was put into the flask and the contents were stirred vigorously. A solution of 183 g (1.0 mole) of 3-vinylbenzene bromide in 500 ml of dried tetrahydrofuran was dropped little by little over 2 hours. The reaction temperature was maintained 75° to 80° C. and, after the addition of the solution, the stirring was continued for further 1 hour as it stands. Into the thus obtained Grignard reagent of 3-vinylphenylmagnesium bromide, a solution of 122.6 g (1.02 mole) of acetophenone in 500 ml of dried tetrahydrofuran was dropped little by little for 2 hours. The reaction temperature was maintained at 75° to 80° C. and, after the dropping, the stirring was continued for further 1 hour as it stands. The reaction mixture was then poured into 3 liter of an aqueous solution of 75 g of ammonium chloride and it was left to stand still for 20 hours and an oily layer was recovered to obtain 1-(3-vinylphenyl)-1-phenylethyl alcohol (VPA: formula (IV)) in a yield 89% (acetophenone basis) by distilling off the tetrahydrofuran.
WORKUP
后处理
- customTo a 2 liter three-neck flask equipped with a dropping funnel, a reflux condenser and a stirrer
- customwas dried sufficiently
- dry with materialAfter that, 50 ml of tetrahydrofuran which has been dried with a molecular sieve 5A
- temperatureThe reaction temperature was maintained 75° to 80° C.
- additionafter the addition of the solution
- temperatureThe reaction temperature was maintained at 75° to 80° C.
- waitafter the dropping, the stirring was continued for further 1 hour as it
- waitwas left
- waitto stand still for 20 hours
- customan oily layer was recovered