DIETHYL 2-(2-NITROBENZYL)MALONATE synthesis

6synthesis methods

Product Name:DIETHYL 2-(2-NITROBENZYL)MALONATE
CAS Number:59803-35-9
Molecular formula:C14H17NO6
Molecular Weight:295.29

3958-60-9 Synthesis

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Yield:59803-35-9 63%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl-formamide at 20; for 2 h;Inert atmosphere;

Steps:

7.7.1.a

To a stirred solution of diethylmalonate (8.89 g, 0.055 mol) in dimethylformamide (50 ml_), potassium carbonate (9.6 g, 0.069 mol) was added and it was stirred for 15 minutes in an inert atmosphere. 1-(bromomethyl)-2-nitrobenzene (10 g, 0.046 mol) in dimethylformamide (10 ml_) was added to the reaction mixture. The reaction mixture was stirred at ambient temperature for 2 hours. TLC showed the total consumption of the starting material. The reaction mixture was diluted with water (600 mL) and the aqueous part was extracted with ethyl acetate (3 x 250 mL). The organic part was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel: 100-200 mesh, eluent: 5% ethyl acetate in hexane) to afford the pure compound (8.7g, 63% yield).

References:

WO2010/127855,2010,A1 Location in patent:Page/Page column 145

17455-13-9 Synthesis