These common heterocyclic compound, 74534-15-9, name is 1-Chloro-2-iodo-4-nitrobenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 1-Chloro-2-iodo-4-nitrobenzene
The experimental operation was performed in a G20 argon-filled oxygen-free anhydrous glove box, and the compound was added to a 250 ml sealed tube10 (2.0 g, 7.06 mmol), Compound 11 (2.3 g, 9.17 mmol), KoAC (2.1 g, 21.2 mmol), PdCl2 (dppf) (464.6 mg, 0.64 mmol) and DMF (dimethylformamide, 32 ml) Stir at room temperature until dissolved, tighten the stopper and fill the tube with argon, move the sealed tube into the silicone oil bath, and react at 65C for 15 hours.Continue in the glove box and continue to cool to room temperature. Continue to add compound 13 (4.78g, 21.2mmol), CS2CO3 (6.9g, 21.2mmol) and double distilled water (16ml) to the sealed tube. Tighten the stopper and remove the gloves. The box was stirred at 60C for 3 hours, and the reaction was completed by TLC monitoring.After cooling to room temperature, the oil pump was spin-dried, and extracted with dichloromethane/water. The product was in the organic phase, and the organic phase was separated and dried over anhydrous Na2SO4. The organic solvent was removed by spin-drying to obtain the crude product. Column chromatography, petroleum ether: Elution with ethyl acetate = 70: 1 gave compound 203 as a white solid, 203 mg, overall yield over two steps: 3.2%.
The synthetic route of 1-Chloro-2-iodo-4-nitrobenzene has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Tianjin International Bio-pharmaceutical Joint Institute; Yang Cheng; Rao Zihe; Bai Cuigai; Sun Tao; Li Mingwei; Li Huiying; Li Xiaohui; Lu Jun; Zhao Xiujuan; Sun Tongyan; (41 pag.)CN107556289; (2018); A;,
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