反应详情

温度

140 °C

To a solution of 500 mg 5-Nitro-3-trimethylsilanylethynyl-pyridin-2-ylamine in 4 ml ethanol were added 93.5 mg sodium hydroxide, and the mixture was stirred under irradiation in a microwave-oven for 30 minutes (min) at 140° C. 20 equal batches of this kind were combined and evaporated. The residue was dissolved in 100 ml conc. hydrochloric acid and stirred for 30 min at RT. It was again evaporated and the residue was refluxed with THF for 30 min. Insoluble parts were removed by filtration, the filtrate was evaporated and the residue was chromatographed on silica in ethyl acetate/heptane mixtures.

1. customevaporated
2. dissolutionThe residue was dissolved in 100 ml conc. hydrochloric acid
3. stirringstirred for 30 min at RT
4. customIt was again evaporated
5. temperaturethe residue was refluxed with THF for 30 min
6. customInsoluble parts were removed by filtration
7. customthe filtrate was evaporated
8. customthe residue was chromatographed on silica in ethyl acetate/heptane mixtures