Scheme 1.
Synthesis of rotaxane 1 H⋅3 PF6. Reagents and conditions: A) CH3CN, NH4PF6, reflux, 18 h, 50 %; B) 4-carboxy-TEMPO (5), DMAP, DCC, CH2Cl2, rt, 24 h, 70 %; C) CHCl3, NH4PF6, reflux, 4 d, 30%.
Synthesis of rotaxane 1 H⋅3 PF6. Reagents and conditions: A) CH3CN, NH4PF6, reflux, 18 h, 50 %; B) 4-carboxy-TEMPO (5), DMAP, DCC, CH2Cl2, rt, 24 h, 70 %; C) CHCl3, NH4PF6, reflux, 4 d, 30%.