反应详情

To a stirred and cooled (−78° C.) solution of bromide 4 (0.20 g, 0.64 mmol) in Et2O (2.5 mL) was added dropwise a 1.5 M solution of tert-BuLi in pentane (0.89 mL, 1.34 mmol). After 38 min MeI (0.1 mL, 1.61 mmol) was added dropwise and the mixture allowed to gradually warm to r.t. After 12 h the mixture was partitioned between CHCl3 and saturated aqueous NaHCO3 solution. The aqueous layer was extracted with CHCl3 (2×). The combined organic extracts were dried (MgSO4), and concentrated to afford 7 as a yellow oily residue, which was used directly in the next step without purification.

1. customAfter 12 h the mixture was partitioned between CHCl3 and saturated aqueous NaHCO3 solution
2. extractionThe aqueous layer was extracted with CHCl3 (2×)
3. dry with materialThe combined organic extracts were dried (MgSO4)
4. concentrationconcentrated
5. customto afford 7 as a yellow oily residue, which
6. customwas used directly in the next step without purification