反应详情

To a stirred and cooled (−90° C.) solution of bromide 4 (206 mg, 0.66 mmol) in THF (2.5 mL) was added dropwise 1.5 M solution of tert-butyllithium in pentane (1 mL, 1.51 mmol). After 35 min additional stirring at −90° C., tri-n-butyltin iodide (0.23 mL, 0.79 mmol) was added in one portion. The mixture was stirred at −90° C. for 10 min, −78° C. for 40 min, and then allowed to warm to r.t. The mixture was partitioned between AcOEt-brine. The aqueous layer was extracted with AcOEt (3×) and the combined organic solutions were dried (MgSO4), and concentrated to afford the crude stannane 17, which was used in the next step without purification.

1. stirringAfter 35 min additional stirring at −90° C.
2. stirringThe mixture was stirred at −90° C. for 10 min, −78° C. for 40 min
3. customThe mixture was partitioned between AcOEt-brine
4. extractionThe aqueous layer was extracted with AcOEt (3×)
5. dry with materialthe combined organic solutions were dried (MgSO4)
6. concentrationconcentrated