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CAS No. : | 16859-59-9 | MDL No. : | MFCD00956142 |
Formula : | C8H6O3 | Boiling Point : | 362.6°C at 760 mmHg |
Linear Structure Formula : | - | InChI Key : | N/A |
M.W : | 150.13 g/mol | Pubchem ID : | 3804259 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With sodium methylate In methanol at 0 - 20℃; for 1 h; | Dimethyl phosphite (11 g, 0.1 mol) at 0 ° CAdd dropwise to a solution of sodium methoxide in methanol (100 ml).Then 2-carboxy benzaldehyde (10.5g, 0.05mol)Add to the reaction system,The entire process temperature is controlled below 5 °C.Thereafter, the mixture was heated to room temperature for 1 hour.Methanesulfonic acid (10.6 g, 0.11 mol) was added.The reaction solution was concentrated and washed with water and chloroform.The organic layers were combined and dried over anhydrous NaSO4.Concentrated to:3-oxo-1,3-dihydroxy-isobenzofuran-1-phosphate dimethyl ester (16 g),The yield was 95percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | Stage #1: at 0 - 20℃; for 1 h; Stage #2: With methanesulfonic acid In methanol |
Dimethyl phosphite (22.0 g, 0.2 mol) was added drop-wise to a solution of sodium methoxide (43.0 g) in methanol (100 ml) at 0oC. 2- Carboxybenzaldehyde (21.0 g, 0.1 mol) was then added portion-wise to the reaction mixture as a slurry in methanol (40 ml), with the temperature kept below 5oC. The resulting pale yellow solution was warmed to 20oC over 1 hour. Methanesulphonic acid (21.2 g, 0.22 mol) was added to the reaction drop-wise and the resulting white suspension was evaporated in vacuo. The white residue was quenched with water and extracted into chloroform (3 x 100 ml). The combined organic extracts were washed with water (2 x 100 ml), dried over MGSO4, and evaporated in vacuo to yield (3-OXO-1, 3-dihydro-isobenzofuran-1-yl) phosphonic acid dimethyl ester as a white solid (32.0 g, 95 percent, 95 percent purity). This was then used without further purification in the next stage |
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