反应详情

Diphenylacetonitrile (17.1 g) was added to a stirred suspension of sodium hydride (4 g of a 60% suspension in mineral oil) in anhydrous toluene (250 ml) and the mixture was heated under reflux for 2 hours. On cooling to room temperature, 1-tosyl-3-(R,S)-tosyloxypyrrolidine (28 g - see Preparation 5) was added in portions and the mixture heated under reflux for 3 hours. The mixture was diluted with toluene (150 ml), washed with 5% aqueous sodium hydroxide (2×100 ml) and brine (150 ml) then dried (MgSO4) and concentrated in vacuo to give a solid which was purified by trituration with methanol to give the title compound as a colourless microcrystalline powder, yield 18 g, m.p. 186°-187° C.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 2 hours
3. temperaturethe mixture heated
4. temperatureunder reflux for 3 hours
5. washwashed with 5% aqueous sodium hydroxide (2×100 ml) and brine (150 ml)
6. dry with materialthen dried (MgSO4)
7. concentrationconcentrated in vacuo
8. customto give a solid which
9. customwas purified by trituration with methanol