HRID851879

反应详情

EQUATION

反应方程式

HRID 851879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Acetonitrile (20 ml), 0.66 mmol of the product of Example 52 and 1.98 mmol of bromotrimethylsilane are stirred at reflux for 1 h. The solvent and the excess of reagent are evaporated off in vacuo and the residue is taken up in solution in 10 ml of methanol. After stirring for 30 min., the solution is evaporated to dryness and the residue is taken up in 1N HCl. A gum is obtained which is crystallised by adding a small amount of CH2Cl2. The expected product is recovered by filtration.

WORKUP

后处理

  1. temperatureat reflux for 1 h
  2. customThe solvent and the excess of reagent are evaporated off in vacuo
  3. customthe solution is evaporated to dryness
  4. customA gum is obtained which
  5. customis crystallised
  6. additionby adding a small amount of CH2Cl2
  7. filtrationThe expected product is recovered by filtration