Table 1.
Performed in PhCl at 40 °C for 40 h using 2 mol % [Co(P2)] under N2 in the presence of 4 Å MS; [azide 1] = 0.1 M; isolated yields.
In situ addition of TMSN3 (1.1 equiv) and TBAF (1.1 equiv).
In situ addition of MeOH (2.0 mL) and H2SO4 (30 mol %).
Absolute configuration was determined by X-ray as (3R, 4S).
At 80 °C for 20 h.
100% conversion; >90% NMR yield.