反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux for 1.25 hours
- customprepared
- stirringThe reaction mixture is stirred
- temperaturewithout cooling for a further 4 hours
- extractionextracted with diethyl ether
- washThe ether phases are washed with water
- dry with materialdried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated