Category: 333447-42-0

333447-42-0, name is 1,5-Difluoro-2-iodo-4-methylbenzene, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Quality Control of 1,5-Difluoro-2-iodo-4-methylbenzene

A solution of 1,5-difluoro-2-iodo-4-methylbenzene (26, 7.11 g, 28.0 mmol), Zn(CN)2 (1.97 g, 16.8 mmol) and Pd(PPh3)4 (3.23 g, 2.8 mmol) in DMF (40 mL) was heated at 90 C for 1.5 h. The reaction mixture was concentrated in vacuo and the residue was taken in water (400 mL) and extracted with ether (400 mL). The combined organic layer was washed with excess aq ammonium hydroxide solution. The separated organic layers were dried and purified b chromatography to yield purified product which contained triphenylphospine oxide. The crude mixture was further purified by sublimation (45 C, 1 mm/Hg) to yield 27 (1.8 g, 42%) as a colorless solid. 1H NMR (400 MHz, CDCl3) delta 7.47 (t, 1H, J = 8.0 Hz), 6.92 (t, 1H, J = 9.2 Hz), 2.27 (s, 3H).

The synthetic route of 333447-42-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Venkatraman, Srikanth; Velazquez, Francisco; Gavalas, Stephen; Wu, Wanli; Chen, Kevin X.; Nair, Anilkumar G.; Bennett, Frank; Huang, Yuhua; Pinto, Patrick; Jiang, Yueheng; Selyutin, Oleg; Vibulbhan, Bancha; Zeng, Qingbei; Lesburg, Charles; Duca, Jose; Heimark, Larry; Huang, Hsueh-Cheng; Agrawal, Sony; Jiang, Chuan-Kui; Ferrari, Eric; Li, Cheng; Kozlowski, Joseph; Rosenblum, Stuart; Shih, Neng-Yang; George Njoroge; Bioorganic and Medicinal Chemistry; vol. 22; 1; (2014); p. 447 – 458;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

333447-42-0, name is 1,5-Difluoro-2-iodo-4-methylbenzene, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 333447-42-0

Step B – Synthesis of Compound 29B; A solution of compound 29A (7.11 g, 28.0 mmol), zinc cyanide (1.97 g, 16.8 mmol) and tetrakis(triphenylphosphine)palladium(0) (3.23 g, 2.80 mmol) in DMF (30 mL) was heated to 90 0C and allowed to stir at this temperature for 1.5 hours. The reaction mixture was concentrated in vacuo and the residue obtained was taken up in water (400 mL) and extracted with ether (400 mL). The organic extract was washed with aqueous ammonium hydroxide solution (IN)- The organic layer was dried (MgSO4) filtered, concentrated in vacuo to provide a residue that was purified using flash column chromatography (SiO2, EtOAc/Hexanes) to provide a mixture that contained product and triphenylphosphine. This mixture was further purified using sublimation at 1 mm/Hg at 45 0C to provide compound 29B (1.8 g; Yield = 42%).

The synthetic route of 333447-42-0 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 333447-42-0, These common heterocyclic compound, 333447-42-0, name is 1,5-Difluoro-2-iodo-4-methylbenzene, 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.

Step B – Synthesis of Compound CC2; A solution of compound CCl (7.11 g, 28.0 mmol), zinc cyanide (1.97 g, 16.8 mmol) and tetrakis(triphenylphosphine)palladium(0) (3.23 g, 2.80 mmol) in DMF (30 mL) was heated to 900C and allowed to stir at this temperature for 1.5 hours. The reaction mixture was concentrated in vacuo and the residue obtained was taken up in water (400 mL) and extracted with ether (400 mL). The organic extract was washed with aqueous ammonium hydroxide solution (IN). The organic layer was dried (MgSO4) filtered, concentrated in vacuo to provide a residue that was purified using flash column chromatography (SiO2, EtOAc/Hexanes) to provide a mixture that contained product and triphenylphosphine. This mixture was further purified using sublimation at 1 mm/Hg at 45 0C to provide compound CC2 (1.8 g; Yield = 42%).

Statistics shows that 1,5-Difluoro-2-iodo-4-methylbenzene is playing an increasingly important role. we look forward to future research findings about 333447-42-0.

Reference:
Patent; SCHERING CORPORATION; WO2008/82484; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com