Abstract Photoaffinity derivatives 7 and 8 of adenophostin A, modified at the 5′-and 1′- positions, were prepared by a chemoselective reaction of the aminophostins 15 and 30 with N-succinimidyl p-benzoyl-2, 3-dihydrocinnamate (p-benzoyldihydrocinnamoyl-N- hydroxysuccinimide; BZDC-NHS, 21). The latter compound was prepared by Heck coupling of 4-iodobenzophenone (16) with methyl acrylate.