反应详情

In a three neck round-bottom flask equipped with a stirring bar, reflux condenser, and rubber septa is placed [1,4′]bipiperidinyl-4′-carboxylic acid amide (5.01 g, 23.7 mmol) in 140 mL of anhydrous 1-propanol and the solution is heated to reflux. Sodium metal (˜9.276 g, 403.4 mmol) rinsed in hexane to remove mineral oil) is added in portions. Once the sodium metal completely dissolves, the mixture is allowed to stir over the weekend. The reaction mixture is cooled to room temperature and the solvent removed under reduced pressure. Distilled water is added and the solution extracted with chloroform. The organic layer is collected, dried over sodium sulfate, filtered, and the solvent removed under reduced pressure to afford 4.4 g of the desired product which is used without further purification. 1H NMR (CD3OD, 300 MHz) δ 1.48–1.60 (m, 8H), 1.72–1.80 (m, 2H), 2.61–2.71 (m, 6H), 2.92–3.01 (m, 2H), 3.37 (s, 1H), 3.56 (s, 2H). MS (ESI) m/z 199 (M+H+).

1. customIn a three neck round-bottom flask equipped with a stirring bar
2. temperaturereflux condenser
3. temperaturethe solution is heated to reflux
4. customto remove mineral oil)
5. additionis added in portions
6. dissolutionOnce the sodium metal completely dissolves
7. customthe solvent removed under reduced pressure
8. additionDistilled water is added
9. extractionthe solution extracted with chloroform
10. customThe organic layer is collected
11. dry with materialdried over sodium sulfate
12. filtrationfiltered
13. customthe solvent removed under reduced pressure