反应详情

To a solution of Example 1B (2.4 g, 0.01 mol) in dry tetrahydrofuran was added n-butyl lithium 4.4 mL, 2.5 M in hexane) at −78° C. drop wise. After stirring at this temperature, tributyltin chloride (3.0 mL, 0.011 mol) was added slowly. The solution was then stirred for 3 hours while warming up to room temperature. Water was added and the solution was extracted with ethyl acetate. The organic layer was washed with sat. NH4Cl, brine, and then dried over magnesium sulfate. The solution was filtered, concentrated, and purified to give 4.85 g of the title compound as a clear oil (93% yield). 1H NMR (300 MHz, CDCl3) δ ppm 0.77-1.74 (m, 33H) 4.40-4.63 (m, 1H) 6.84-6.95 (m, 2H) 7.12 (s, 1H) 7.14 (m, 2H). MS (ESI) m/z 526.2 (M+H)+.

1. additionwas added slowly
2. extractionthe solution was extracted with ethyl acetate
3. washThe organic layer was washed with sat. NH4Cl, brine
4. dry with materialdried over magnesium sulfate
5. filtrationThe solution was filtered
6. concentrationconcentrated
7. custompurified