Synthesis of the Spermidine/Spermine series of N-alkylpolyamines
Reagents:
a. (i)CH2=CHCN, MeOH, r.t, 15h; (ii) Boc2O (excess), MeOH, r.t, 12h.
b. AcOH, Pd(OH)2/C, H2, 50 psi; Boc2O (excess), MeOH, r.t, 12h.
c. (i) 1,4-Diaminobutane (excess), Pd(OH)2/C, H2, 60 psi; (ii) Boc2O (excess), MeOH, r.t, 12 h.
d. CF3CO2H (excess), r.t.
e. (i) CF3COOEt (1or 2 Eq.), MeOH. −78°C to 0° C, 1h; (ii) Boc2O (excess); (iii) LiOH, THF, r.t.
f. (i) CH2=CHCN (2 Eq.), MeOH, r.t, 15 h; (ii) Boc2O (excess), MeOH, r.t, 12h.
g. AcOH, Pd(OH)2/C, H2, 50 psi; Boc2O (excess), MeOH, r.t, 12 h.
h. NaH, C16H33I, DMF, −15°C-r.t, 24h.