HRID746197

反应详情

EQUATION

反应方程式

HRID 746197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The procedure of Example 1 was repeated, except that there was utilized 16.9 grams (0.70 mole) of magnesium metal and 100 grams (0.66 mole) of 4-chloro-α-methylstyrene dissolved in 200 ml. of tetrahydrofuran. The Grignard reaction was started by the addition of a small amount of methyl iodide. After the reaction mixture had been refluxed for 12 hours, there was added at 0° C. in a dropwise manner a solution of 85 grams of t-butylperbenzoate in 300 ml. of ethylether. A crystalline product identified as 4,4'-diisopropenylbiphenyl was isolated from the oil which was recovered by filtering the mixture and washing with methanol. After stripping the methanol, a 69.3% yield of 4-t-butoxy-α-methylstyrene was isolated by fractional distillation as a colorless liquid having a boiling point of 65°-68° C. at 0.03 millimeters.

WORKUP

后处理

  1. dissolutiondissolved in 200 ml
  2. customThe Grignard reaction
  3. temperatureAfter the reaction mixture had been refluxed for 12 hours
  4. customwas isolated from the oil which
  5. customwas recovered
  6. filtrationby filtering the mixture
  7. washwashing with methanol