反应详情

To a solution of [2,2,2-Trifluoro-1-(2-fluoro-phenyl)-eth-(Z)-ylidene]-carbamic acid tert-butyl ester (16.63 g, 57.1 mmol) in 170 mL THF at −75° was added dropwise allylmagnesium chloride solution 2 mol/L in THF (31.4 ml, 62.8 mmol). The reaction temperature was not allowed to exceed −60° C. After 30 minutes, the reaction was quenched with 10% aqueous NH4Cl and extracted with TBME. The organic phase was washed with brine, dried with MgSO4.H2O and evaporated. The crude product was chromatographed on silica gel with hexane/TBME 95/5 to give 18.52 g of the title compound.

1. customto exceed −60° C
2. customthe reaction was quenched with 10% aqueous NH4Cl
3. extractionextracted with TBME
4. washThe organic phase was washed with brine
5. dry with materialdried with MgSO4.H2O
6. customevaporated
7. customThe crude product was chromatographed on silica gel with hexane/TBME 95/5