反应详情

According to the General Procedure using 4-hydroxybenzoic acid (80 mg, 0.58 mMol), dicyclohexylcarbodiimide (125 mg, 0.61 mMol), and spermine (430 mg, 2.13 mMol) in DME/DMF (4 ml, 3:1), activation during 3 h and coupling over 48 h. The product was eluted over silica gel with dichloromethane/methanol/0.880 ammonia solution (2:2:1). The desired amide was in fractions 8-12 and was homogeneous when monitored by tic on silica (CH2Cl2 /MeOH/NH4OH, 2:2:1), Rf =0.29, (23 mg, 12%), lyophilisation gave 7 mg of a colourless, viscous oil whose spectroscopic data include: pmr (90 MHz, 2H2O) 1.4-1.9 (m, 8H, 4×CH2 --CH2), 2.5-2.9 (m, 10H, 5×CH2 --N), 3.25 (t, J=7, 2H, CON2H--CH2 --CH2) 6.6-6.9 (m, 2H, 2×ArH 3,5), and 7.0-7.3 (m, 2H, 2×ArH2,6)ppm; M+1 323 (FAB matrix m-nitrobenzyl alcohol) C17H30N4O2 requires M+ 322).

1. customduring 3 h
2. washThe product was eluted over silica gel with dichloromethane/methanol/0.880 ammonia solution (2:2:1)
3. customgave 7 mg of a colourless, viscous oil whose spectroscopic data