反应详情

温度

80 °C

A mixture of 2-methoxy-4-nitrophenol (0.207 mg. 1.23 mmole) {Aldrich}, methyl 4-bromo-3-methylbutyrate(0.25 g. 1.35 mmole) and potassium carbonate (0.19 g. 1.35 mmole) in DMF (10 mL.) was heated and stirred at 80° C. for 8 hours. After cooling, the inorganics were filtered off, and the filtrate evaporated to dryness. The residue was dissolved in dichloromethane and washed twice with water. After drying (MgSO4) the solvent was evaporated off to yield an oil. The oil was purified by chromatography (Varian Megabondelut silica column) using a gradient of 100% dichloromethane to 20% ethyl acetate/dichloromethane to give methyl 3-methyl-4-(2-methoxy-5-nitrophenoxy)butyrate as an oil (90 mg. 29%) ms 284(M+)

1. temperaturewas heated
2. temperatureAfter cooling
3. filtrationthe inorganics were filtered off
4. customthe filtrate evaporated to dryness
5. dissolutionThe residue was dissolved in dichloromethane
6. washwashed twice with water
7. dry with materialAfter drying (MgSO4) the solvent
8. customwas evaporated off
9. customto yield an oil
10. customThe oil was purified by chromatography (Varian Megabondelut silica column)