HRID971831

反应详情

EQUATION

反应方程式

HRID 971831 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
16 °C

PROCEDURE

实验过程

Into a 250 ml flask equipped with a magnetic stirring bar, addition funnel and calcium sulfate drying tube is placed a solution of 10.84g (0.06 mole, 98.66% pure) of 2,5-dimethyl-2,5-dihydroperoxyhexane in 120 ml of anhydrous ether. The solution is cooled to 16° C. and a solution of 8.77g (0.06 mole) of bis(dimethylamino) dimethylsilane in 30 ml of anhydrous ether is added slowly dropwise. The reaction temperature is maintained between 15° and 20° by use of an ice bath and by adjusting the rate of addition. After the addition is complete, the solution is stirred at room temperature for one hour. The solution is filtered to remove a small amount of suspended solid. The solvent is removed by distillation yielding 13.75g of 3,3,6,6,9,9-hexamethyl-1,2,4,5-tetraoxa-3-silacyclononane (theoretical yield 14.05g, 97.9%; A.O. analysis 13.32%, theoretical 13.67%, 97.4% pure). The infrared spectrum of the reaction product of this example is identical to the spectrum of material produced in Example 1.

WORKUP

后处理

  1. customInto a 250 ml flask equipped with a magnetic stirring bar, addition funnel and calcium sulfate drying tube
  2. temperatureThe reaction temperature is maintained between 15° and 20° by use of an ice bath
  3. additionthe rate of addition
  4. additionAfter the addition
  5. filtrationThe solution is filtered
  6. customto remove a small amount of suspended solid
  7. customThe solvent is removed by distillation