Dimethyl 5-nitroisophthalate synthesis
- Product Name:Dimethyl 5-nitroisophthalate
- CAS Number:13290-96-5
- Molecular formula:C10H9NO6
- Molecular Weight:239.18
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In a 100 mL three-necked round-bottomed flask equipped with a condenser tube, an electric stirrer and a thermometer, 5.0 g of 5-nitroisophthalic acid and 33.3 mL of methanol were added sequentially. The mixture was stirred under nitrogen protection at room temperature for about 3 minutes until the solid was completely dissolved to give a colorless transparent solution. Subsequently, 1.0 mL of concentrated sulfuric acid was slowly added dropwise and heated to reflux, and after the reaction for about 3 hours, white solid precipitation was observed. The progress of the reaction was monitored by thin layer chromatography (TLC, unfolding agent ratio of dichloromethane:methanol=10:1). Upon completion of the reaction, it was cooled to room temperature, crystals were precipitated and the solid product was collected by filtration. The filter cake was washed with deionized water and finally mixed with a small amount of water and dried to obtain dimethyl 5-nitroisophthalate. The product yield was 98%.
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Yield:13290-96-5 98%
Reaction Conditions:
with sulfuric acid for 3 h;Inert atmosphere;Reflux;
Steps:
1 Example 1. Synthesis of 5 - Nitroisophthalic Acid Dimethyl Ester
In a 100 mL round bottom flask equipped with a condenser, an electric stirrer and a thermometer5.0 g of 5-nitroisophthalic acid,Add 33.3ml of methanol, in the case of N2, stirring at room temperature, 3min or so, the solid completely dissolved, the solution colorless and clear and transparent, and then slowly add 1.0ml concentrated sulfuric acid, heating reflux, about 3h white solid precipitation, TLC (CH2Cl2: CH3OH = 10: 1), cooled, crystallized, filtered, washed with a small amount of water and the filter cake was dried to give dimethyl 5-nitroisophthalate. The yield was 98%.
References:
CN105254521,2016,A Location in patent:Paragraph 0025
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