反应详情

A mixture comprising of 3,5-dichlorobenzyl 4-(2-aminoethyl)piperidine-1-carboxylate (Example 3, step 1) (100 mg, 0.302 mmol), 2-(1H-1,2,3-triazol-4-yl)acetic acid (57.6 mg, 0.453 mmol), 1-propanephosphonic anhydride solution (0.353 mL, 0.604 mmol) and Huenig's Base (0.105 mL, 0.604 mmol) in DMF (1 mL) was stirred at room temperature for 18 hours, and then concentrated under reduced pressure. The mixture was diluted with water and extracted with EtOAc. The organic portion was dried over MgSO4, filtered and the solvent concentrated under 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. concentrationconcentrated under reduced pressure
2. additionThe mixture was diluted with water
3. extractionextracted with EtOAc
4. dry with materialThe organic portion was dried over MgSO4
5. filtrationfiltered
6. concentrationthe solvent concentrated under 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