反应详情

According to the General Procedure using 3-Hydroxybenzoic acid (138 mg, 1.00 mMol), dicyclohexylcarbodiimide (226 mg, 1.10 mMol), and spermine (400 mg, 1.98 mMol) in dichloromethane (6 ml), activation during 3 h and coupling over 17 h. The product was eluted over silica gel with dichloromethane/methanol/0.880 ammonia solution (4:2:1). The desired amide was in fractions 8-13 was homogeneous when monitored by tlc on silica (CH2Cl2 /MeOH/NH4OH, 4:2:1), Rf =0.29, (76 mg, 24%), lyophilisation gave 52 mg of a colorless, 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), 6.5-6.8 (m, 3H, 3× ArH 2,4,6), and 7.0-7.3 (m, 1H, ArH 5) ppm; M+1 323 (FAB matrix m-nitrobenzyl alcohol and sodium chloride) C17H30N4O2 requires M+ 322).

1. customduring 3 h
2. washThe product was eluted over silica gel with dichloromethane/methanol/0.880 ammonia solution (4:2:1)
3. customgave 52 mg of a colorless, viscous oil whose spectroscopic data