Dimethyl malonate → Dimethyl-3-nitrobiphenyl-4-malonate

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 stirred 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 stirred 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 washed with water and brine and evaporated to give a yellow oil, crude dimethyl-3-nitrobiphenyl-4-malonate.

1. customwas ,cooled to room temperature
2. stirringThe mixture was stirred at 100° C. for 2 hours
3. temperaturecooled
4. customquenched with 300 ml of saturated ammonium chloride solution
5. extractionThe mixture was extracted three times with ethyl acetate
6. washthe combined organic layers washed with water and brine
7. customevaporated

ORD-Eintrag

ord-1f4029578bd042bc97cea44af58e39a1

Quelldatensatz

uspto-grants-2005_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06855730B2