反应详情

To a solution of 2-(3-iodo-pyrrolo[3,2-c]pyridine-1-yl)-propionic acid methyl ester (Preparation 57, 18.1 g, 54.8 mmol) in EtOH (300 mL) was added 2M lithium borohydride solution in THF (63.1 mL, 126 mol) at 0° C. The reaction was stirred at this temperature for 30 minutes before warming to room temperature for 18 hours. The reaction was quenched by the addition of water (300 mL) at 0° C. with stirring for 1 hour. The EtOH was removed in vacuo and the resulting residue diluted further with water (600 mL) followed by extraction into 5% MeOH in DCM (250 mL). The organic layer was collected, dried over MgSO4 and concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 0-5% MeOH in DCM to afford the title compound (12 g, 73%).

1. customThe reaction was quenched by the addition of water (300 mL) at 0° C.
2. stirringwith stirring for 1 hour
3. customThe EtOH was removed in vacuo
4. additionthe resulting residue diluted further with water (600 mL)
5. extractionfollowed by extraction into 5% MeOH in DCM (250 mL)
6. customThe organic layer was collected
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo
9. customThe residue was purified
10. washeluting with 0-5% MeOH in DCM