DIMETHYL 2-METHYL-2-(4-NITROPHENYL)MALONATE synthesis
- Product Name:DIMETHYL 2-METHYL-2-(4-NITROPHENYL)MALONATE
- CAS Number:131675-32-6
- Molecular formula:C12H13NO6
- Molecular Weight:267.23
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Yield:131675-32-6 66%
Reaction Conditions:
with potassium carbonate in N,N-dimethyl-formamide at 0 - 23; for 18 h;
Steps:
A155.2
Step 2: To a stirred solution of dimethyl 2-(4-nitrophenyl)malonate (10 g, 39.52 mmol, 1 .0 eq) and K2C03 (10.9 g 79.05 mmol 2.0 eq ) in DMF (40 mL), was added methyl iodide (4.94 mL, 79.05 mmol 2.0 eq) at 0 °C and the mixture stirred at RT for 18h. K2C03 was filtered off and the filtrate concentrated under vacuum. The residue was diluted with water (80 mL) and extracted with EtOAc (2 x 80 mL). The organic layer was separated washed with brine solution, dried over anhydrous Na2S04 and the solvent evaporated to get dimethyl 2-methyl-2-(4-nitrophenyl)malonate(7 g, 66%; TLC system: EtOAc/PE (3:7), Rf: 0.5.)
References:
WO2013/68461,2013,A1 Location in patent:Page/Page column 141
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