反应详情

(E)-2-(6-chloro-3-iodo-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)-N,N-dimethylethenamine (1.0 g, 1.692 mmol) and ethanamine HCl (0.552 g, 6.77 mmol) were stirred in a 3:1:1 solution of DCE:AcOH:EtOH (5 ml) at 100° C. for 2 hrs. Solvent was removed by vacuum and the residue was taken in DCE (15 ml) and treated with sodium triacetoxyborohydride (0.9 g, 4.23 mmol), acetic acid (0.4 g, 6.7 mmol) and stirred at room temperature for 6 hours. The eaction mixture was partitioned between DCM and aqueous sodium bicarbonate and the organics was separated, washed with brine, dried with sodium sulfate and concentrated. Purification of the residue by flash column (0-15% MeOH-DCM) gave 2-(6-chloro-3-iodo-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)-N-ethylethanamine. MS ESI calc'd. for C29H26ClIN4 [M+H]+ 593. found 593.

1. customSolvent was removed by vacuum
2. customThe eaction mixture was partitioned between DCM and aqueous sodium bicarbonate
3. customthe organics was separated
4. washwashed with brine
5. dry with materialdried with sodium sulfate
6. concentrationconcentrated
7. customPurification of the residue by flash column (0-15% MeOH-DCM)