Реакция #77402

Уравнение реакции

4-fluoro-3-nitrobiphenyl

Dimethyl malonate

sodium hydride

→

dimethyl-3-nitrobiphenyl-4-malonate

Растворители

dimethylsulfoxide

dimethylsulfoxide

dimethylsulfoxide

Условия реакции

Обработка

1. 1
   ТемператураThe mixture was cooled to room temperature
2. 2
   ТемператураThe mixture was heated at 100° C. for 2 hours
3. 3
   Температураcooled
4. 4
   Другоеquenched with 300 mL of saturated ammonium chloride solution
5. 5
   ЭкстракцияThe mixture was extracted three times with ethyl acetate
6. 6
   Промывкаthe combined organic layers were washed with water and brine
7. 7
   Другоеevaporated

Методика

Dimethyl malonate (10 mL) in 25 mL of dimethylsulfoxide was added dropwise to 3.5 g of sodium hydride suspended in 25 mL of dimethylsulfoxide and the mixture heated at 100° C. for 10 minutes. The mixture was cooled to room temperature and 4.7 g of 4-fluoro-3-nitrobiphenyl in 25 mL of dimethylsulfoxide was added. The mixture was heated at 100° C. for 2 hours, cooled and quenched with 300 mL of saturated ammonium chloride solution. The mixture was extracted three times with ethyl acetate and the combined organic layers were washed with water and brine and evaporated to give crude dimethyl-3-nitrobiphenyl-4-malonate as a yellow oil.

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