反应详情

A mixture comprising of 3,5-dichlorobenzyl 4-(2-(methylamino)ethyl)piperidine-1-carboxylate (Example 1, step 3) (100 mg, 0.290 mmol), 2-(1H-1,2,3-triazol-4-yl)acetic acid (55.2 mg, 0.434 mmol), T3P® (50% solution in DMF) (338 μl, 0.579 mmol) and Huenig's base (101 μl, 0.579 mmol) in DMF was stirred at room temperature for 18 hours. The resulting mixture was concentrated under pressure. The crude residue was diluted with water and extracted with EtOAc. The organic portion was dried over MgSO4, filtered and solvent concentrated under reduced pressure. Further purification was carried out using preparative LC-MS. The resulting product fractions were concentrated under reduced pressure to give an aqueous solution and then extracted with EtOAc. The organic extracts were dried over MgSO4, filtered and concentrated under reduced pressure to afford the title compound.

1. concentrationThe resulting mixture was concentrated under pressure
2. additionThe crude residue was diluted with water
3. extractionextracted with EtOAc
4. dry with materialThe organic portion was dried over MgSO4
5. filtrationfiltered
6. concentrationsolvent concentrated under reduced pressure
7. customFurther purification
8. concentrationThe resulting product fractions were concentrated under reduced pressure
9. customto give an aqueous solution
10. extractionextracted with EtOAc
11. dry with materialThe organic extracts were dried over MgSO4
12. filtrationfiltered
13. concentrationconcentrated under reduced pressure