反应详情

温度

50 °C

A 100 ml two-necked round-bottomed flask equipped with a KPG-stirrer, a thermometer and a reflux condenser is charged with ethanol (50 ml), water (5 ml), iron (1.43 g) and hydrochloric acid 37% (0.2 ml). The reaction mixture is heated at 50° C. 2-(3-tert-Butyl-phenoxy)-3-methyl-5-nitro-pyridine (2.26 g) was added portionwise. The mixture is heated at reflux for 3 hours. After cooling the mixture to 50° C. it is filtered through celite. The filtrate is poured into water (200 ml) and extracted with ethylacetate (2×50 ml). The combined organic layers are washed with brine (100 ml), dried over sodium sulfate, filtered and the solvent is removed in vacuo. Purification by flash chromatography over silica gel with hexane/ethyl acetate 1:1 (v:v) gives 1.10 g of the compound as a brownish solid (MP: 83-84° C.).

1. customA 100 ml two-necked round-bottomed flask equipped with a KPG-stirrer
2. temperatureThe mixture is heated
3. temperatureat reflux for 3 hours
4. temperatureAfter cooling the mixture to 50° C. it
5. filtrationis filtered through celite
6. additionThe filtrate is poured into water (200 ml)
7. extractionextracted with ethylacetate (2×50 ml)
8. washThe combined organic layers are washed with brine (100 ml)
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. customthe solvent is removed in vacuo
12. customPurification by flash chromatography over silica gel with hexane/ethyl acetate 1:1 (v:v)