反应详情

To a solution of 1,1-dimethylethyl 4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl)-1-piperidinecarboxylate (i.e. the product of Step A) (0.815 g, 1.97 mmol) in dichloromethane (50 mL) was added a solution of hydrogen chloride and diethyl ether (2 M, 10 mL, 20 mmol). The reaction mixture was stirred at room temperature for 1 h to give a gummy precipitate. Methanol was added to dissolve the precipitate, and the reaction mixture was stirred for an additional 1 h. The reaction mixture was concentrated under reduced pressure and partitioned between ethyl acetate and saturated aqueous sodium bicarbonate, the organic layer was dried (MgSO4) and concentrated to give the title compound as a clear oil (0.31 g), which solidified on standing.

1. customto give a gummy precipitate
2. dissolutionto dissolve the precipitate
3. stirringthe reaction mixture was stirred for an additional 1 h
4. concentrationThe reaction mixture was concentrated under reduced pressure
5. custompartitioned between ethyl acetate and saturated aqueous sodium bicarbonate
6. dry with materialthe organic layer was dried (MgSO4)
7. concentrationconcentrated