反应详情

To a solution of Example 32 (0.99 g, 2.75 mmol) in dry tetrahydrofuran (50 mL) was added methyl magnesium bromide (4.58 mL of a 3M solution in ether, 13.7 mmol). The solution was heated at reflux for 75 minutes, quenched with 5% aqueous potassium hydrogen sulfate and extracted with ethyl acetate and the organic phase was washed with brine, dried (magnesium sulfate) and evaporated. The residue was combined with the product of a previous reaction (0.55 mmol scale) to afford 1.26 g of off-white foamy solid. Chromatography on silica (flash; 75% ethyl acetate/hexanes) afforded 0.28 g (24%) of Example 35 as a white foamy solid (melting point 97°-101° C.) as well as 0.40 g of slightly less pure material.

1. temperatureThe solution was heated
2. temperatureat reflux for 75 minutes
3. customquenched with 5% aqueous potassium hydrogen sulfate
4. extractionextracted with ethyl acetate
5. washthe organic phase was washed with brine
6. dry with materialdried (magnesium sulfate)
7. customevaporated
8. customThe residue was combined with the product of a previous reaction (0.55 mmol scale)