反应详情

Approximately 400 mg of Raney nickel is added to a mixture of 2.84 g (15.9 mmol) of 1-methyl-5-nitroindoline and 4 ml (80 mmol) of hydrazine hydrate in-60 ml of absolute ethanol. The reaction mixture is heated to reflux for 5 hours. After returning to 23° C., a little silica is added to the flask and the solvent is evaporated off under vacuum. The evaporation residue is placed directly at the top of a chromatography column. The expected product is eluted using a Heptane/AcOEt mixture (3/7). A violet powder is obtained (65%) which is used directly in the following stage.

1. temperatureThe reaction mixture is heated
2. temperatureto reflux for 5 hours
3. customAfter returning to 23° C.
4. additiona little silica is added to the flask
5. customthe solvent is evaporated off under vacuum
6. washThe expected product is eluted
7. customA violet powder is obtained (65%) which