反应详情

温度

80 °C

To the filtrate obtained in the above crude (3R)-3-aminopyrrolidine D(-)-tartrate is added a solution of L(+)-tartaric acid (25 g) in water (50 ml), and the precipitated crystals are separated by filtration. The product is dissolved in a 20% aqueous sodium hydroxide solution (50 ml) and thereto is added acetone (300 ml), and the precipitated crystals are removed by filtration. To the filtrate is added a solution of L(+)-tartaric acid (20 g) in water (40 ml). The precipitated crystals are separated by filtration and dissolved in water (30 ml), and thereto is added sodium hydroxide (300 g). The mixture is extracted with ether (300 ml) three times. Ether is distilled off under reduced pressure, and to the residue is added a solution of L(+)-tartaric acid (5.5 g) in water (25 ml), and the mixture is heated at 80° C. To the mixture is added methanol (40 ml), and the mixture is gradually cooled till room temperature. The precipitated crystals are separated by filtration and recrystallized from a mixed solvent of methanol-water (1:1) to give (3S)-3-aminopyrrolidine L(+)tartrate (5.0 g).

1. customthe precipitated crystals are separated by filtration
2. dissolutionThe product is dissolved in a 20% aqueous sodium hydroxide solution (50 ml)
3. additionis added acetone (300 ml)
4. customthe precipitated crystals are removed by filtration
5. additionTo the filtrate is added a solution of L(+)-tartaric acid (20 g) in water (40 ml)
6. customThe precipitated crystals are separated by filtration
7. dissolutiondissolved in water (30 ml)
8. additionis added sodium hydroxide (300 g)
9. extractionThe mixture is extracted with ether (300 ml) three times
10. distillationEther is distilled off under reduced pressure
11. additionto the residue is added a solution of L(+)-tartaric acid (5.5 g) in water (25 ml)
12. additionTo the mixture is added methanol (40 ml)
13. temperaturethe mixture is gradually cooled till room temperature
14. customThe precipitated crystals are separated by filtration
15. customrecrystallized from a mixed solvent of methanol-water (1:1)