[CH2:1]([O:3][C:4]([C:6]1([F:13])[CH2:11][CH2:10][CH2:9][NH:8][C:7]1=[O:12])=[O:5])[CH3:2]>C(O)C>[F:13][C@@:6]1([C:4]([O:3][CH2:1][CH3:2])=[O:5])[CH2:11][CH2:10][CH2:9][NH:8][C:7]1=[O:12]Samples were prepared in batches according to the following method: ethyl-3-fluoro-2-oxo-3-piperidinecarboxylate (25 g) was dissolved in ethanol (450 ml) with gentle heating and sonication. The solution was then filtered through a Pall Acrodisc 37 mm syringe filter with 1 μm glass fibre membrane to remove fines and undissolved material. The filtered solution was adjusted to a total volume of 500 ml with ethanol to give a solution with nominal concentration of 50 mg/mL.
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