Dimethyl aminoterephthalate synthesis

6synthesis methods

Product Name:Dimethyl aminoterephthalate
CAS Number:5372-81-6
Molecular formula:C10H11NO4
Molecular Weight:209.2

5292-45-5 Synthesis

5292-45-5
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$6.00/5g

5372-81-6
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$17.67/5gm:

Yield:5372-81-6 99.1%

Reaction Conditions:

with iron;ammonium chloride in ethanol;water; for 0.5 h;Reflux;Solvent;

Steps:

1.2

Nitro Reduction: To 50ml volume ratio of 1: 1 ethanol / water solution of ammonium chloride was added 2.3g, iron 2.3g, stirred heated to reflux for 30min; 2-nitro-dimethyl terephthalate (ie, compound II ) 10.0 g was dissolved in 25ml of ethanol, was added dropwise to the reaction flask slowly (to prevent the red material), after the addition was complete the reaction was continued at this temperature for 30min, TLC monitored the reaction was complete; cooled to room temperature, filtered through celite pad, the cake washed with until no product was adsorbed was washed with ethanol, and concentrated under reduced pressure to remove ethanol; aqueous layer was washed with saturated Na₂CO₃Solution was adjusted pH10, 50mlEA aqueous phase was extracted twice, the combined organic phase was washed by saturated sodium chloride, dried over anhydrous sodium sulfate, and evaporated to dryness to give 8.7g solid, i.e., 2-amino dimethyl terephthalate (i.e. compound III ), shown in Figure 2, a yield of 99.1%,

References:

CN104072403,2016,B Location in patent:Paragraph 0034

67-56-1 Synthesis