反应详情

In this reference example, 5.24 g of 1-benzyl-4-amino-piperidine dihydrochloride, 3.02 g of o-nitrobenzaldehyde, 2.02 g of triethylamine and 30 ml of methanol are mixed and stirred at room temperature for one hour. The resultant solution is cooled with ice and stirred. To the stirred solution, 1 g of sodium borohydride is added little by little over a period of one hour. Then, the mixture is brought back to room temperature and stirred at room temperature for 2 hours. The resultant solution is poured into 200 ml of ice water and extracted with ether. The organic layer is washed with water, dried and concentrated. The oily residue is dissolved in 20 ml of ethanol. The solution is mixed with 10 ml of a solution of 5.7 N hydrochloric acid in ethyl acetate. The white crystals deposited are separated by filtration, washed with 20 ml of ethyl acetate and dried to obtain 5.70 g of a crude product. The crude product is recrystallized from hot ethanol to obtain 2.90 g of the desired product.

1. stirringstirred
2. customis brought back to room temperature
3. stirringstirred at room temperature for 2 hours
4. extractionextracted with ether
5. washThe organic layer is washed with water
6. customdried
7. concentrationconcentrated
8. dissolutionThe oily residue is dissolved in 20 ml of ethanol
9. additionThe solution is mixed with 10 ml of a solution of 5.7 N hydrochloric acid in ethyl acetate
10. customThe white crystals deposited are separated by filtration
11. washwashed with 20 ml of ethyl acetate
12. customdried
13. customto obtain 5.70 g of a crude product
14. customThe crude product is recrystallized from hot ethanol