Rapid and facile one-step microwave synthesis of macrobicyclic cryptands.

Liquid-assisted grinding (LAG) and microwave synthesis are proposed as alternative routes for the synthesis of cryptands, with reaction times of up to 16 times faster than traditional methods. These rapid and facile techniques have the potential to replace traditional methods for a high-yield formation of clathrochelates, and other materials. The cryptand 6,16,25-tribenza-1,4,8,11,14,18,23,27-octa-aza-tri-cyclo-[9.9.9]nona-cosa-4,7,14,17,23,26-hexaene hexa-hydrate, C(36)H(42)N(8)·6H(2)O, (Ph(3)T(2) ) was synthesized using this novel method. The crystal structure was redetermined by single-crystal X-ray diffraction using synchrotron radiation at 120†K. The structure exhibits disorder in the water mol-ecule of hydration.