反应详情

To a degassed solution of the product from Step 2 (0.30 g, 0.77 mmol), 18-Crown-6 (102 mg, 0.39 mmol), and Bu4NI (28 mg, 0.077 mmol) in THF at −78° C. was added the KOtBu solution. After 15 min. at −78° C., a solution of di(tert-butyl)(4-(bromomethyl)phenyl)(difluoro)methyl phosphonate (Example 1, Step 7) (319 mg, 0.77 mmol) in THF (3 mL) via double-tipped needle. The cold bath was removed and the reaction was stirred at r.t. for 1.5 h. Saturated NH4Cl solution was then added and the product was extracted with EtOAc. The organic layer was washed with H2O and brine, and was then dried (MgSO4), filtered, and evaporated. The residue was purified by flash chromatography (1:20 Et2O: toluene, 1% Et3N) to give an oil (98 mg).

1. customThe cold bath was removed
2. additionSaturated NH4Cl solution was then added
3. extractionthe product was extracted with EtOAc
4. washThe organic layer was washed with H2O and brine
5. dry with materialwas then dried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by flash chromatography (1:20 Et2O: toluene, 1% Et3N)