反应详情

Into a round bottom flask were placed 2.00 g (9.1 mmol) of 3-pyrrolidinone benzyl carbamate, from Example 1 Step 2, dissolved in 40 mL of toluene, 1.65 mL (22.8 mmol) of 1,3-propanediol and 0.09 g (0.46 mmol) of p-toluenesulfonic acid. The mixture was heated at 110°-125° C. for 48 hours. The solution was poured into 100 mL of 5% sodium bicarbonate solution, and the product was extracted into ethyl acetate, which was then dried over anhydrous sodium sulfate. The solvent was removed under vacuum, and the residue distilled in a kugelrohr apparatus (200° C. @ 2.5 Torr) to afford the title compound, MS: M/Z 295 (M+NH4), which was taken directly to the next step.

1. customInto a round bottom flask were placed
2. temperatureThe mixture was heated at 110°-125° C. for 48 hours
3. extractionthe product was extracted into ethyl acetate, which
4. dry with materialwas then dried over anhydrous sodium sulfate
5. customThe solvent was removed under vacuum
6. distillationthe residue distilled in a kugelrohr apparatus (200° C. @ 2.5 Torr)