反应详情

1.77 g (0.005 mol) of the resulting trans-3-hydroxy-4-phenoxy-1-(β,β,β-trichloroethoxycarbonyl)-pyrrolidine are dissolved in 20 ml of 90% strength acetic acid and the solution is treated at 0° with 2 g of zinc dust in portions. The reaction mixture is then stirred at room temperature for one hour and filtered through a layer of diatomaceous earth and the filtrate is rendered alkaline with concentrated sodium hydroxide solution and extracted 3 times with ether. The organic phase is washed with water, dried over calcium chloride and evaporated under a water pump vacuum, and trans-3-hydroxy-4-phenoxy-pyrrolidine is obtained in the form of the crude base, which crystallises from methylene chloride/hexane; melting point 120°-122°. The neutral fumarate of this compound, which has a melting point of 144°-146°, is obtained by reaction with a solution of fumaric acid in methanol/ether.

1. filtrationfiltered through a layer of diatomaceous earth
2. extractionextracted 3 times with ether
3. washThe organic phase is washed with water
4. dry with materialdried over calcium chloride
5. customevaporated under a water pump vacuum