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Preparation of 3 and 5 To ice-cold 1 (0.95 g, 2.75 mmol) in CH2Cl2 (anhyd, 20 mL) was added oxalyl chloride (0.25 mL, 3.03 mmol, followed by DMF (0.005 mL) under N2 and the mixture stirred for 0.5 h. p-Xylenediamine (0.169 mg, 1.24 mmol) and DIPEA (0.48 mL, 2.75 mmol) were stirred together in the presence of 4 Å MS in CH 2Cl2 (anhyd, 10 mL) until complete dissolution of the amine. The solution containing the acid chloride was added, and the mixture was stirred for a further 2 h at 0 ° C. The mixture was extracted with CH 2Cl2 (20 mL, washed with NaHCO3 (2 x 15 mL, HCl (2 x 15 mL, brine (2 x 15 mL, H2O (2 x 15 mL, dried (Na 2SO4, filtered, and the solvent removed to give a pale brown foam. Silica gel chromatography (EtOAc-Cy, gradient elution, 1:1 to 2:1) gave the protected diamide as a white foam (0.359 g, 37, This diamide 74
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For a recent application of cyclophanes, see: Yoon, I.; Benitez, D.; Zhao, Y.-L.; Miljanic, O. S.; Kim, S.-Y.; Tkatchouk, E.; Leung, K. C.-F.; Khan, S. I.; Goddard, W. A. III.; Stoddart, J. F. Chem. Eur. J. 2009, 15, 1115.
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