反应详情

温度

50 °C

A 250 ml two-necked round-bottomed flask equipped with a KPG-stirrer, a thermometer and a reflux condenser is charged with ethanol (100 ml), water (10 ml), iron (3.11 g) and hydrochloric acid 37% (0.3 ml). The reaction mixture is heated at 50° C. 2-(4-chloro-3-trifluoromethyl-phenoxy)-3-methyl-5-nitro-pyridine (5.81 g) is added portionwise. The mixture was heated at reflux for 2 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 to obtain 4.20 g of the compound as yellow solid (MP: 92-94° C.).

1. customA 250 ml two-necked round-bottomed flask equipped with a KPG-stirrer
2. temperatureThe mixture was heated
3. temperatureat reflux for 2 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