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Reagents and conditions: (a) (i) 10% aq HCl, NaNO2; (ii) NaN3; (b) 1-decyne, sodium ascorbate, CuSO4, t-BuOH/H2O (1:1), 12 h, rt; (c) acetylenic substrate (24, 1-hexyne; 25, 1-heptyne; RB-056, 1-decyne), sodium ascorbate, CuSO4, t-BuOH, H2O; (d) MsCl, Et3N, CH2Cl2, 0 °C to rt, 5 h; (e) piperidine, MeCN (RB-059–RB-061), 1-methylpiperidine, MeCN (RB-060–RB-062) or 4-hydroxypiperidine, MeCN, 50 °C, 12 h (RB-063–RB-065).
