反应详情

To a refluxing mixture of [2-(5-chloro-2-nitrophenyl)-1-(4-methoxyphenyl)ethyl]propanedioic acid, dimethyl ester (40 g, 95.0 mmole) and hydrated ferrous sulfate (184.5 g, 0.663 mole) in a (1:10 solution of methanol:water (1.2 L) was added concentrated ammonium hydroxide (142.5 ml) over a 30 minute period. The reaction was stirred at reflux for 20 minutes then cooled to room temperature. Ethyl acetate and Celite were added and the mixture was filtered through Celite. The filtrate was partitioned between ethyl acetate and water. The organic phase was dried over magnesium sulfate and concentrated in vacuo. The product was recrystallized from isopropyl alcohol to yield 28.22 g of the title compound, melting point 114°-116° C.

1. temperatureat reflux for 20 minutes
2. filtrationthe mixture was filtered through Celite
3. customThe filtrate was partitioned between ethyl acetate and water
4. dry with materialThe organic phase was dried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe product was recrystallized from isopropyl alcohol