反应详情

The starting material is prepared as follows: The mixture of 10 g of 2-(2-tosyloxyethyl)-1,4-benzodioxan, 10 g of 4-piperidone hydrochloride, 20 g of anhydrous sodium carbonate and 160 ml of dimethylformamide is stirred vigorously at room temperature for 48 hours. It is filtered, the residue washed with a small amount of dimethylformamide and the filtrate evaporated. The residue is dissolved in ethyl acetate, the solution extracted with hydrochloric acid, the extract made alkaline with 50% aqueous sodium hydroxide while cooling and re-extracted with methylene chloride. The latter extract is dried and evaporated, to yield the 2-[2-(4-oxopiperidino)-ethyl]-1,4-benzodioxan, which solidifies on standing.

1. customThe starting material is prepared
2. filtrationIt is filtered
3. washthe residue washed with a small amount of dimethylformamide
4. customthe filtrate evaporated
5. dissolutionThe residue is dissolved in ethyl acetate
6. extractionthe solution extracted with hydrochloric acid
7. temperaturewhile cooling
8. extractionre-extracted with methylene chloride
9. extractionThe latter extract
10. customis dried
11. customevaporated