反应详情

To a solution of (3-hydroxy-3-methyloctyl)(triphenyl)phosphonium iodide (800 mg) in anhydrous tetrahydrofuran (9.00 mL) was added n-butyllithium (1.60M in hexane, 1.90 mL) at room temperature and the solution was stirred for 1 Hour. To the solution was added a solution of the compound 49 (349 mg) in anhydrous tetrahydrofuran (6.00 mL) was slowly added at −78° C. and the solution was stirred for 2 Hours. The solution temperature was risen to room temperature. The reaction solution was poured into ice water and extracted with ethyl acetate. The organic layer was washed water and brine, dried over anhydrous sodium sulfate and concentrated. The obtained residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=4:1) to give the title compound (178 mg) having the following physical data.

1. additionwas slowly added at −78° C.
2. stirringthe solution was stirred for 2 Hours
3. customwas risen to room temperature
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed water and brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated
8. customThe obtained residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=4:1)