Ethyl isonicotinate synthesis
- Product Name:Ethyl isonicotinate
- CAS Number:1570-45-2
- Molecular formula:C8H9NO2
- Molecular Weight:151.16
Yield:1570-45-2 97.2%
Reaction Conditions:
with pyrographite in toluene at 130; for 0.166667 h;Irradiation;Claisen Condensation;
Steps:
1.1; 2.1; 3.1 (1) Preparation of ethyl 4-pyridinecarboxylate
0.8 mol of isonicotinic acid was added in sequence to a 100 mL three-necked flask.0.64 mol of absolute ethanol, 2.0 g of activated powdered activated carbon was used as a catalyst, and toluene was used as a solvent.The microwave reaction time was 10 min (power 200 W; temperature 130 ° C).The reaction solution was neutralized with a saturated aqueous solution of Na 2 CO 3 until the pH was 7, and the layer was allowed to stand, and the upper layer was taken;The aqueous phase was extracted with 20 mL of chloroform and combined with organic layer.The chloroform was recovered by atmospheric distillation and then distilled under reduced pressure to give a colorless transparent liquid ethyl 4-pyridinecarboxylate with a purity of 96.3% (GC) and a yield of 97.2%.
The activated powdery activated carbon was obtained by immersing the powdered activated carbon in 60 mL of a 25% aqueous solution of p-toluenesulfonic acid for 30 hours, suction filtration, and drying.
References:
Zhengzhou Changkuan Technology Co., Ltd.;Business Qiu Polytechnic College;Lv Haikuan;Liu Bing;Zhang Haiyang;Du Zifei;Zheng Chaochao CN109535067, 2019, A Location in patent:Paragraph 0039; 0060-0063; 0070-0073; 0080-0083
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