反应详情

A mixture of 2.30 g (0.02 mol) of 3-(hydroxymethyl)piperidine, 5.5 ml (0.04 mol) of triethylamine and 4.90 g (0.02 mol) of 2-(3,4-dimethoxy-phenyl)-ethyl bromide is refluxed for 2 hours. After cooling, the reaction mixture is dissolved in a mixture of 2 molar sodium hydroxide solution and methylene chloride. The organic phase is washed with water, separated off, dried over magnesium sulphate, evaporated down in vacuo and purified over 300 g of aluminium oxide (neutral, activity II-III) with methylene chloride and then with increasing amounts of ethanol (up to 2%). Yield: 4.4 g (78.7% of theory), Melting point: 87.5°-89° C.

1. temperatureis refluxed for 2 hours
2. temperatureAfter cooling
3. washThe organic phase is washed with water
4. customseparated off
5. dry with materialdried over magnesium sulphate
6. customevaporated down in vacuo
7. custompurified over 300 g of aluminium oxide (neutral, activity II-III) with methylene chloride