反应详情

温度

60 °C

A solution of 3,3-dimethyl-6-nitro-1,3-dihydro-indol-2-one (6 g, 29.10 mmol) in anhydrous N,N-dimethylformamide (DMF) (35 ml) was treated with sodium hydride. The resulting suspension was stirred for 1 h at 60° C. A solution of bromo-ethane (2.17 mL, 3.17 g, 29.10 mmol) in DMF (10 ml) was added. The mixture was allowed to cool to room temperature and stirred for 1 h. After removal of the solvent the mixture was quenched with water (100 ml) and extracted with ethyl acetate (3×100 ml). The extract was dried over Na2SO4, evaporated and the crude product was purified by column chromatography on silica gel. Elution with ethyl acetate/n-heptane (1:3) yielded 5.94 g (87%) of a yellow solid.

1. temperatureto cool to room temperature
2. stirringstirred for 1 h
3. customAfter removal of the solvent the mixture
4. customwas quenched with water (100 ml)
5. extractionextracted with ethyl acetate (3×100 ml)
6. dry with materialThe extract was dried over Na2SO4
7. customevaporated
8. customthe crude product was purified by column chromatography on silica gel
9. washElution with ethyl acetate/n-heptane (1:3)