反应详情

温度

70 °C

A mixture of 1-(diphenylmethyl)-3-methyl-3-azetidinyl methanesulfonate (1.55 g, 4.68 mmol) (J. Med. Chem. 1993, 36, 801-810) and pyrrolidine (3.86 ml, 46.68 mmol) in isopropanol (15 ml) was heated to 70° C. overnight. After cooling to room temperature, the mixture was concentrated to dryness in vacuo. Water (100 ml) was added, and the mixture was extracted with dichloromethane (2×100 ml). The combined organic solution was washed with brine (60 ml), dried (Na2SO4) and concentrated. The residue was purified via RP-HPLC to provide 1-[1-(diphenylmethyl)-3-methyl-3-azetidinyl]pyrrolidine (0.94 g, 65%). LCMS: (M+H)+: 307.2.

1. temperatureAfter cooling to room temperature
2. concentrationthe mixture was concentrated to dryness in vacuo
3. additionWater (100 ml) was added
4. extractionthe mixture was extracted with dichloromethane (2×100 ml)
5. washThe combined organic solution was washed with brine (60 ml)
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe residue was purified via RP-HPLC