反应详情

5-(1H-1,2,3-Triazol-4-yl)entanoic acid (step 3) (50 mg, 0.294 mmol) and 3,5-dichlorobenzyl 4-aminopiperidine-1-carboxylate hydrochloride (Example 17, step 2) (100 mg, 0.294 mmol) were dissolved in DMF (1 ml). DIPEA (257 μl, 1.472 mmol) was added followed by 50% T3P® solution in DMF (344 μl, 0.589 mmol). The reaction mixture was stirred at RT for 96 hrs and concentrated under reduced pressure. The crude product was dissolved in DCM and washed with 10% citric acid. The organic portion was separated, dried over MgSO4 (anh), filtered and evaporated under reduced pressure. Purification by preparative HPLC afforded product fractions that were concentrated to afford a residue. The residue was dissolved in DCM and washed with a minimal volume of water, dried over MgSO4 (anh) filtered and evaporated under reduced pressure to afford the title compound;

1. concentrationconcentrated under reduced pressure
2. dissolutionThe crude product was dissolved in DCM
3. washwashed with 10% citric acid
4. customThe organic portion was separated
5. dry with materialdried over MgSO4 (anh)
6. filtrationfiltered
7. customevaporated under reduced pressure
8. customPurification by preparative HPLC
9. customafforded product fractions that
10. concentrationwere concentrated
11. customto afford a residue
12. washwashed with a minimal volume of water
13. dry with materialdried over MgSO4 (anh)
14. filtrationfiltered
15. customevaporated under reduced pressure