反应详情

According to Example 15, 3-methylpyrrolidin-3-ol hydrochloride was synthesized. To a 100 mL reaction flask were added 3-methylpyrrolidin-3-ol hydrochloride (1 g, 7.2 mmol), anhydrous potassium carbonate (2.5 g, 18 mmol) and acetonitrile (15 mL). To the resulting mixture was slowly added a solution of 2-bromoethylbenzene (1.2 g, 6.48 mmol) in acetonitrile dropwisely at 85° C. The reaction was conducted for 12 hours. After the completion of reaction monitored by TLC, the resulting mixture was evaporated under reduced pressure to remove acetonitrile. To the residue was added a mixed solution of dichloromethane and water for extraction. The organic phase was dried over anhydrous sodium sulfate, and evaporated to remove the solvent to produce a crude product. The crude product was purified by column chromatography (silica gel column, eluted with petroleum ether:ethyl acetate=30:1 (volumetric ratio)) to produce 3-methyl-1-phenylethylpyrrolidin-3-ol (1 g) in a yield of 75.2%.

1. customwas synthesized
2. customTo a 100 mL reaction flask
3. customAfter the completion of reaction
4. customthe resulting mixture was evaporated under reduced pressure
5. customto remove acetonitrile
6. additionTo the residue was added a mixed solution of dichloromethane and water
7. extractionfor extraction
8. dry with materialThe organic phase was dried over anhydrous sodium sulfate
9. customevaporated
10. customto remove the solvent
11. customto produce a crude product
12. customThe crude product was purified by column chromatography (silica gel column, eluted with petroleum ether:ethyl acetate=30:1 (volumetric ratio))