PHOSPHONIC ACID, ETHYL METHYL ESTER synthesis
- Product Name:PHOSPHONIC ACID, ETHYL METHYL ESTER
- CAS Number:1610-33-9
- Molecular formula:C3H9O3P
- Molecular Weight:124.08
Yield:1610-33-9 78.4 %Spectr.
Reaction Conditions:
Stage #1: Ethylphosphorige Saeurewith phosphorus pentoxide in acetonitrile at 52; for 2 h;Inert atmosphere;
Stage #2: methanol in acetonitrile at 53; for 0.166667 h;Inert atmosphere;
Steps:
13 General procedure for the synthesis of diesters of phosphorous acid.
General procedure: In a three-necked round-bottom flask, equipped with a mechanical stirrer, a reflux condenser and a dosing funnel, under nitrogen atmosphere, is added the first P-O component (PIII-OH). This first P-O component (table 1 column 5) is selected from H3PO3, monoalkyl phosphites or a mixture thereof and may further comprise dialkyl phosphites. The first P-O component is then heated to the temperature as given in table 1, column 11 (T° Step a) before proceeding to step a). The second P-O component (table 1 column 6) is then added while the temperature is maintained appropriately. The mixture is then allowed to react during the period of time, as given in table 1 column 13 (Reaction time step a) before proceeding to step b). Alcohol R1-OH (table 1 column 3) is then added dropwise while the temperature is maintained at the temperature as given in table 1 column 12 (T° Step b). The mixture is then allowed to react during the period of time, as given in table 1 column 14 (Reaction time b) before cooling down to room temperature and performing 31P NMR analysis.
References:
EP2581378,2013,A1 Location in patent:Paragraph 0038; 0039; 0043
