Scheme 4a.
aConditions: (a) Ac2O, NaOAc, reflux, 1 h, 62%; (b) PhSH, BF3·Et2O, CHCl3, rt, 5 h, 82%; (c) LiOH, MeOH, rt, 1 h; NH4Cl, rt, 20 min; (d) 2-methoxypropene, CSA, DMF, rt, 3 h, 82% (2 steps); (e) lithium naphthalenide, THF, −78°C, 30 min, >99%; (f) NaH, MeI, THF, rt, 2 h, 81%; (g) t-BuLi, THF, −78 °C to 0 °C, 30 min then Me2SiHCl, −78°C to rt, 1 h, 44%.