反应详情

A solution of (R)-6-(3-(4-bromophenyl)-3-o-tolylpropanoyl)-2-methylpyridazin-3(2H)-one (example 8, step 3; 235 mg, 571 μmol), and p-toluenesulfonic acid monohydrate (10.9 mg, 57.1 μmol) in 2-ethyl-2-methyl-1,3-dioxolane (2.33 g, 20.0 mmol) was heated for 45 min at 110° C., then partitioned between sat. aq. sodium hydrogencarbonate solution and ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate, filtered, and evaporated. Chromatography (SiO2; gradient heptane-ethyl acetate) produced the title compound (42 mg, 16%). White semisolid, MS: 455.1 [M+H]+.

1. custompartitioned between sat. aq. sodium hydrogencarbonate solution and ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customevaporated