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A new free-radical initiator, azobisisobutanol diacetate, has been prepared from azobisisobutyronitrile in good yield in three steps: ( 1 ) methanolysis to convert the nitrile groups to ester functions; (2) reduction of the diester to a diol; and (3) acetylation, Thus, it is more easily synthesized than other azo compounds having similar free-radical-generating properties and may be easily tagged with Cl4 if desired. Steady production of free radicals at 167" was demonstrated.

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