反应详情

39.0 g (88.1 mmol) 3-(6-tert-Butoxycarbonylamino-pyridin-3-yl)-2-(1-cyclohexyl-1H-imidazol-4-yl)-propionic acid ethyl ester as prepared in process step b) were suspended in 200 ml Ethanol (EtOH) at RT. The mixture was saturated with HCl and was then refluxed for 2 h. The mixture was concentrated and the residue was treated with saturated aqueous K2CO3 (pH 9.0). The aqueous layer was extracted with AcOEt (3×200 ml). The combined organic layers were washed with brine (100 ml), dried with MgSO4 and concentrated to yield the title compound (30 g, 87.6 mmol, 99%) as brown oil.

1. temperaturewas then refluxed for 2 h
2. concentrationThe mixture was concentrated
3. additionthe residue was treated with saturated aqueous K2CO3 (pH 9.0)
4. extractionThe aqueous layer was extracted with AcOEt (3×200 ml)
5. washThe combined organic layers were washed with brine (100 ml)
6. dry with materialdried with MgSO4
7. concentrationconcentrated