反应详情

温度

180 °C

85.0 g (340 mmol) of 1-benzyl-3-hydroxy-3-(2-hydroxyethylaminomethyl)-pyrrolidine are dissolved in a mixture of 280 ml of concentrated sulfuric acid and 140 ml of water and heated at 180° C. overnight. The mixture is made alkaline with 45% strength sodium hydroxide solution, precipitated salts are dissolved in water, and the solution is extracted five times with 200 ml of chloroform each time. The organic phases are dried over potassium carbonate, the desiccant is removed, and the solution is concentrated. The residue is distilled under high vacuum. 60.0 g (76% of theory) of the product are obtained.

1. customprecipitated salts
2. dissolutionare dissolved in water
3. extractionthe solution is extracted five times with 200 ml of chloroform each time
4. dry with materialThe organic phases are dried over potassium carbonate
5. customthe desiccant is removed
6. concentrationthe solution is concentrated
7. distillationThe residue is distilled under high vacuum
8. custom60.0 g (76% of theory) of the product are obtained