反应 #607474
ord-8a1ea0f3bdd44598bdefa03f3c68ff30
反应方程式
4,4′-trimethylene dipiperidine bispropanoic acid bis-boc-1,3-diamino propane
HCl
→
product
收率 122.7%
4,4′-trimethylene dipiperidine bispropanoic acid 1,3-diamino propane
收率 122.7%
溶剂
反应条件
温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他After removal of the solvent under reduced pressure
- 2workup.DISSOLUTIONthe residue was dissolved in 10 mL of methanol/water (1:1)
- 3workup.ADDITIONwas treated with 5 g of Amberlyst OH 26 resin
- 4workup.STIRRINGAfter stirring at room temperature for 3 hours
- 5过滤the resin was filtered off
- 6其他The filtrate was evaporated dryness
实验过程
To 0.55 g of 4,4′-trimethylene dipiperidine bispropanoic acid-bis-boc-1,3-diamino propane dissolved in 5 mL of methanol was added 0.5 mL of concentrated HCl and the reaction mixture was stirred at 50° C. for 10 hours. After removal of the solvent under reduced pressure, the residue was dissolved in 10 mL of methanol/water (1:1) and was treated with 5 g of Amberlyst OH 26 resin. After stirring at room temperature for 3 hours, the resin was filtered off. The filtrate was evaporated dryness and the residue was lyophilized yielding 0.5 g of the product as a white solid.