反应详情

In 7.0 mL of ethyl acetate was dissolved 1.12 g of tert-butyl=1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-pyrrolidinylcarbamate, and 1.86 mL of 6 mol/L hydrochloric acid was added to the solution, after which the resulting mixture was heated under reflux for 1 hour. After the reaction mixture was cooled, water and ethyl acetate were added thereto and the pH was adjusted to 10 with a 2 mol/L aqueous sodium hydroxide solution, and the organic layer was separated. The organic layer was washed with water and then a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent. The residue was purified by a column chromatography (eluent; chloroform:methanol=30:1 to 20:1) to obtain 0.38 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-pyrrolidinamine as a light-yellow oil.

1. additionwas added to the solution
2. temperatureafter which the resulting mixture was heated
3. temperatureunder reflux for 1 hour
4. temperatureAfter the reaction mixture was cooled
5. customthe organic layer was separated
6. washThe organic layer was washed with water
7. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
8. distillationdistilled under reduced pressure
9. customto remove the solvent
10. customThe residue was purified by a column chromatography (eluent; chloroform:methanol=30:1 to 20:1)