反应详情

温度

70 °C

Iron powder (448 mg, 8.0 mmol) was added to a mixture of ethyl 1-((5-bromo-2-nitrophenylamino)methyl)cyclopropanecarboxylate (684 mg, 2.0 mmol), ammonium chloride aqueous (6 mL) and ethanol (20 mL). The reaction was heated to 70° C. and maintained at the 70° C. for 2 hours. The mixture solution was filtered. The filtrate was evaporated, diluted with water (100 mL), extracted with ethyl acetate (100 mL), and dried by sodium sulfate. The mixture was filtered. The filtrate was concentrated and purified by column chromatography (silica gel, petroleum ether/ethyl acetate=5:1) to give ethyl 1-((2-amino-5-bromophenylamino)methyl)cyclopropanecarboxylate (474 mg, 76%) as off-white solid.

1. temperaturemaintained at the 70° C. for 2 hours
2. filtrationThe mixture solution was filtered
3. customThe filtrate was evaporated
4. additiondiluted with water (100 mL)
5. extractionextracted with ethyl acetate (100 mL)
6. dry with materialdried by sodium sulfate
7. filtrationThe mixture was filtered
8. concentrationThe filtrate was concentrated
9. custompurified by column chromatography (silica gel, petroleum ether/ethyl acetate=5:1)