反应详情

In an argon stream, 2.2 g of 60% sodium hydride was suspended in 20 ml of N,N-dimethylformamide. The suspension was added dropwise to a solution of 9.6 g of the 3-(1-piperidinomethyl)phenol obtained in Reference Example 1 in 30 ml of N,N-dimethylformamide, followed by stirring at room temperature for 30 minutes. Next, a solution of 14.7 g of N-(3-bromopropyl)phthalimide in 50 ml of N,N-dimethylformamide was added dropwise to the mixture, and the resulting mixture was stirred at 65° C. for 8 hours. After cooling the mixture, a mixture of diethyl ether and water (1:1) was added thereto for extraction, and the organic layer was concentrated under reduced pressure. To the concentrate was added 6N hydrochloric acid for extraction into the aqueous layer, which was then made alkaline with potassium hydroxide, followed by extraction with diethyl ether. The organic layer was dried over magnesium sulfate and distilled under reduced pressure to remove the solvent, giving 16.3 g of transparent oily N-[3-[3-(piperidinomethyl)-phenoxy]propyl]phthalimide (yield 86% ).

1. stirringthe resulting mixture was stirred at 65° C. for 8 hours
2. temperatureAfter cooling the mixture
3. additionwas added
4. extractionfor extraction
5. concentrationthe organic layer was concentrated under reduced pressure
6. additionTo the concentrate was added 6N hydrochloric acid
7. extractionfor extraction into the aqueous layer, which
8. extractionfollowed by extraction with diethyl ether
9. dry with materialThe organic layer was dried over magnesium sulfate
10. distillationdistilled under reduced pressure
11. customto remove the solvent