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CAS No. : | 6384-92-5 | MDL No. : | |
Formula : | C5H9NO4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HOKKHZGPKSLGJE-GSVOUGTGSA-N |
M.W : | 147.13 | Pubchem ID : | 22880 |
Synonyms : |
N-Methyl-D-aspartic acid
|
Chemical Name : | (R)-2-(Methylamino)succinic acid |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; In water;Heating / reflux; | Compound 76a:; To a 5.5 N HCI solution (11 mL) of 4-fluoro-1 ,2-phenylene diamine (1.32 g, 10.9 mmol) was added N- methyl-D-aspartic acid (2.00 g, 13.6 mmol). The mixture was refluxed for overnight. It was filtered after cooling down to room temperature. The filtrate was washed with ethyl acetate (10 mL) and EPO <DP n="56"/>concentrated to give the title compound. 1H NMR (CD3OD): delta 7.88 (1 H, dd, J=9.1 , 4.3Hz), 7.65 (1 H, dd, J=8.1 , 2.5Hz), 7.47 (1 H, td, 'J=9.4, 4.3Hz), 4.74 (1 H, dd, J=10.5, 4.5Hz), 4.09 (1 H, dd, J=15.3, 4.4Hz), 3.81 (1H, dd, J=15.2, 10.5Hz), 2.98 (3H, s). LCMS (APCI): 238.1 (M+H+). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62.2 g | With cation exchange resin;pH 2.0; | (5) Preparation of N-methyl-D-aspartic acid:In the reaction vessel, N-methyl-D-aspartate calcium was added,With a regenerated cation exchange resin,So that N-methyl-D-aspartic acid calcium dissolved,And adjust the PH value of 2.0,The cation exchange resin column was charged to collect the effluent,And the pH of the effluent from the resin column was 4 when washed with no ion water,The collection is terminated, the collection liquid is decompressed, concentrated to a slurry,Washed with ethanol, filtered,Dried to give 62.2 g of N-methyl-D-aspartic acid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70.92% | With palladium on activated charcoal; water; In methanol; at 30 - 50℃; for 0.08333330000000001h;Autoclave; | Add 20g to a 250ml stainless steel autoclaveN-methyl-benzyl-aspartate,56 g of methanol and 30 g of purified water were stirred for 5 minutes, and the palladium carbon recovered in the previous batch was added for the first time, and the kettle was replaced with nitrogen for 3 times, and then replaced with hydrogen for 3 times.The hydrogen is pressurized to 0.3 to 0.6 MPa, and the temperature is raised to 30 to 50 C to carry out the reaction.Stop the reaction without stopping the pressure, add 40g purified water, filter, palladium charcoal recovery and use, the filtrate is naturally cooled to 0 ~ 10 C for 2h, suction filtration, drying to obtain 8.8g white solid N-methyl-aspartate , the molar yield is 70.92%;The HPLC purity was 99.9%. |
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