反应详情

25 g (0.65 mol) of sodium amide was introduced into 150 ml of xylene and heated to boiling under agitation. Within one hour, 99 g (0.5 mol) of hydroxymethylcyclododecane, dissolved in 750 ml of xylene, was added dropwise to the boiling suspension. To complete the alcoholate formation the mixture was heated for another two hours under reflux. Thereafter 44 g (0.35 mol) of dimethyl sulfate was added dropwise. The reaction mixture was heated under reflux for another four hours and then poured into a mixture of ice and 35 g of sodium hydroxide. The organic phase was washed with water, dried with Na2SO4, and then distilled.

1. temperatureheated
2. additionwas added dropwise to the boiling suspension
3. temperaturewas heated for another two hours
4. temperatureunder reflux
5. temperatureThe reaction mixture was heated
6. temperatureunder reflux for another four hours
7. washThe organic phase was washed with water
8. dry with materialdried with Na2SO4
9. distillationdistilled