HRID986384

反应详情

EQUATION

反应方程式

HRID 986384 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

16 g (0.1 mole) of bromine are added dropwise to 28.2 g (0.1 mole) of 7-(4-chlorophenoxy)-5-hydroxy-5,6,6-trimethyl-hept-1-ene in 200 ml of absolute chloroform at room temperature, with stirring, followed by 13 g (0.1 mole) of quinoline, at -10° C. with cooling. The reaction mixture is stirred at room temperature for a further 2 hours and concentrated in vacuo, the residue is taken up in ether, the mixture is filtered and concentrated again in vacuo and the residue is stirred at 95° C. on a water-bath for 1 hour. The resulting mixture is taken up in ether and filtered and the filtrate is washed with 15% strength hydrochloric acid and then with water, dried over sodium sulphate and freed from the solvent in vacuo. 32.7 g (90% of theory) of 2-bromomethyl-5-[1-(4-chlorophenoxy)-2-methylprop-2-yl]-5-methyl-tetrahydrofuran are obtained as an oil, which can be used in the next stage without further purification. ##STR142##

WORKUP

后处理

  1. temperaturewith cooling
  2. stirringThe reaction mixture is stirred at room temperature for a further 2 hours
  3. concentrationconcentrated in vacuo
  4. filtrationthe mixture is filtered
  5. concentrationconcentrated again in vacuo
  6. stirringthe residue is stirred at 95° C. on a water-bath for 1 hour
  7. filtrationfiltered
  8. washthe filtrate is washed with 15% strength hydrochloric acid
  9. dry with materialwith water, dried over sodium sulphate