HRID259389

反应详情

EQUATION

反应方程式

HRID 259389 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The Grignard reagent prepared in 300 ml of THF from 24 g (1.0 mole) of magnesium and 42 g (0.30 mole) of β-bromostyrene is decanted from excess metal and added dropwise under nitrogen to a solution of 27 g (0.21 moles) of N-methyl glutarimide at 3°- 5°. After 11/2 hrs. at room temperature, the mixture is treated with 250 ml of saturated NH4Cl solution with cooling. The separated aqueous layer is reextracted and the combined THF extracts washed with salt, dried over MgSO4 and freed of solvent. Product is extracted into hot ether and crystallized on cooling to yield white crystals, mp 108°- 112° C.

WORKUP

后处理

  1. customis decanted from excess metal
  2. custom2 hrs
  3. temperaturewith cooling
  4. washthe combined THF extracts washed with salt
  5. dry with materialdried over MgSO4
  6. extractionProduct is extracted into hot ether
  7. customcrystallized
  8. temperatureon cooling
  9. customto yield white crystals, mp 108°- 112° C.