Water → HCID 10132932, compound

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Reaction Steps

The product of Example 1, Step (b), (0.54 g, 0.0020 mole), N-benzylmethylamine (0.29 g, 0.0024 mole) and potassium carbonate (0.33 g, 0.0024 mole) were stirred in dimethylformamide (25 mL) for 10 days at room temperature. The mixture was concentrated in vacuo. Water (25 mL) and ethyl acetate (25 mL) were added to the residue. The layers were separated and the aqueous layer was washed with ethyl acetate (25 mL). The ethyl acetate layer and washes were combined and dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The product was purified by silica gel chromatography to give an oil. The structure was supported by NMR, infrared spectroscopy and elemental analysis (M.W.=356.46+0.15 mole H2O). Analysis: Calcd. for C22H26N2F2•0.15 M H2O): C, 73.57; H, 7.38; N, 7.80; Found: C, 73.57; H, 7.33; N, 7.71.

Provenance & Evidence