反应详情

温度

23 °C

To a solution of ethyl 2,2-dimethylpent-4-ynoate (1.00 g, 6.5 mmol), 2,2-dimethyl-propionyl chloride (0.8 mL, 6.5 mmol), and dichlorobis(triphenylphosphine) palladium(II) (460 mg, 0.65 mmol) in triethylamine (TEA) (12 mL) is added CuI (62 mg, 0.32 mmol). The mixture is stirred at 23° C. for 3 h then partitioned between Et2O and saturated aqueous NH4Cl. The organics are washed with water, dried with MgSO4, filtered, and concentrated in vacuo. The residue is purified by flash chromatography (SiO2, hexanes to 10% EtOAc in hexanes) to give the title intermediate (828 mg, 54%).

1. customthen partitioned between Et2O and saturated aqueous NH4Cl
2. washThe organics are washed with water
3. dry with materialdried with MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue is purified by flash chromatography (SiO2, hexanes to 10% EtOAc in hexanes)