反应详情

A mixture of (R)-2-ethyl-piperazine-1,4-dicarboxylic acid 4-tert-butyl ester 1-(3-bromo-2,6-difluoro-benzyl) ester (226 mg), tetrakis(triphenylphosphine)palladium (56 mg), trimethylboroxine (122 mg) and potassium carbonate (200 mg) in dioxane (5 mL) was heated to reflux with stirring for 6 h. The cooled was mixture was partitioned between water and ethylacetate. The water phase was extracted once with ethylacetate, organic phases were pooled and dried with Na2SO4 to yield after evaporation a dark oil (259 mg). This residue was purified by column chromatography (silica gel; n-hexane/ethylacetate gradient) to yield 160 mg (82%) of a yellow oil. MS (ISP): 416.4 (M+H)+.

1. temperaturewas heated
2. temperatureto reflux
3. customwas partitioned between water and ethylacetate
4. extractionThe water phase was extracted once with ethylacetate, organic phases
5. dry with materialdried with Na2SO4
6. customto yield
7. customafter evaporation a dark oil (259 mg)
8. customThis residue was purified by column chromatography (silica gel; n-hexane/ethylacetate gradient)