HRID486358

反应详情

EQUATION

反应方程式

HRID 486358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4.53 g of magnesium shavings and a granule of iodine are treated with 150 ml of tetrahydrofuran while stirring and gassing with nitrogen. Subsequently, the mixture is treated dropwise within 20 minutes with a solution of 38.4 g of 1-bromo-4-chlorobenzene in 150 ml of tetrahydrofuran and boiled at reflux for 1.25 hours. Thereafter, the reaction mixture is cooled to 0° C. and treated dropwise at 0°-5° C. within 30 minutes with a solution of 35.7 g of 8-[2-(4-oxocyclohexyl)ethyl]-1,4-dioxaspiro[4,5]decane (prepared starting from 4,4'-(1,2-ethane-diyl)bisphenol in analogy to the synthesis of 8-(4-oxocyclohexyl)-1,4-dioxaspiro[4,5]decane described in EP-A-310,067) in 240 ml of tetrahydrofuran. The reaction mixture is stirred without cooling for a further 4 hours, then treated within 10 minutes with 240 ml of 10 percent ammonium chloride solution and extracted with diethyl ether. The ether phases are washed with water, dried over sodium sulphate, filtered and concentrated, there being obtained 1-(4-chlorophenyl)-4-[2-(1,4-dioxa-spiro[4,5]decyl)ethyl]cyclohexanol.

WORKUP

后处理

  1. temperatureat reflux for 1.25 hours
  2. customprepared
  3. stirringThe reaction mixture is stirred
  4. temperaturewithout cooling for a further 4 hours
  5. extractionextracted with diethyl ether
  6. washThe ether phases are washed with water
  7. dry with materialdried over sodium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated