HRID2108239

反应详情

EQUATION

反应方程式

HRID 2108239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customTo a 2 liter three-neck flask equipped with a dropping funnel, a reflux condenser and a stirrer
  2. customwas dried sufficiently
  3. dry with materialAfter that, 50 ml of tetrahydrofuran which has been dried with a molecular sieve 5A
  4. temperatureThe reaction temperature was maintained 75° to 80° C.
  5. additionafter the addition of the solution
  6. temperatureThe reaction temperature was maintained at 75° to 80° C.
  7. waitafter the dropping, the stirring was continued for further 1 hour as it
  8. waitwas left
  9. waitto stand still for 20 hours
  10. customan oily layer was recovered