反应详情

To a solution of [1-(5-bromo-2-fluoro-phenyl)-2,2-difluoro-eth-(Z)-ylidene]-carbamic acid tert-butyl ester (9.61 g, 27.3 mmol) in 114 ml THF at −75° was added dropwise allylmagnesium chloride solution 2 mol/L in THF (15.0 ml, 30 mmol). The reaction temperature was not allowed to exceed −60° C. After 10 minutes the reaction was quenched with 10% aqueous NH4Cl and extracted with TBME. The organic phase was washed with brine, dried with Na2SO4 and evaporated. The crude product was chromatographed on silica gel with 1-5% TBME/hexane to give 10.39 g of the title compound.

1. customto exceed −60° C
2. customAfter 10 minutes the reaction was quenched with 10% aqueous NH4Cl
3. extractionextracted with TBME
4. washThe organic phase was washed with brine
5. dry with materialdried with Na2SO4
6. customevaporated
7. customThe crude product was chromatographed on silica gel with 1-5% TBME/hexane