Diethyl fluoromalonate synthesis
- Product Name:Diethyl fluoromalonate
- CAS Number:685-88-1
- Molecular formula:C7H11FO4
- Molecular Weight:178.16
In a 250m1 round bottom flask, 5g of sodium carbonate, 10g of cobalt octacarbonyl, 72ml (57g, 1. 25mol) of ethanol and 53ml (61g, 0. 5mol) of ethyl chloroacetate were added, and CO2 was passed through the gas at a flow rate of 50m1/min for 6h, and the
105-53-3
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685-88-1
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Yield:685-88-1 85%
Reaction Conditions:
with triethylamine pentahydrogen fluoride salt;iodosylbenzene in 1,2-dichloro-ethane at 70; for 24 h;Reagent/catalyst;Concentration;
Steps:
Fluorination of Malonic Esters 1; General Procedure
General procedure: PhIO (550 mg, 2.5 mmol), Et3N·5HF (800 mg, 4 mmol), and DCE (1 mL)were placed in a Teflon test tube. After stirring at r.t. for 15 min, the appropriate malonic ester 1 (1 mmol) and DCE (1 mL) were added. The test tube was sealed with a septum rubber and heated at 70 °C for 24 h with stirring. The reaction mixture was neutralized with aq NaHCO3 and the product was extracted with CH2Cl2 (3 × 10 mL). The combined organic layers were washed with brine (20 mL), dried (Na2SO4), and concentrated under reduced pressure. The product was purified by column chromatography on silica gel with hexane-CH2Cl2 as eluent.
References:
Kitamura, Tsugio;Muta, Kensuke;Oyamada, Juzo [Synthesis,2015,vol. 47,# 20,art. no. SS-2015-F0334-OP,p. 3241 - 3245]
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685-88-1
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