Category: 723294-75-5

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 723294-75-5 as follows. Application In Synthesis of 3-Fluoro-5-iodobenzonitrile

A mixture of compound 1 (15mg, 0.085mmol), compound 2(25mg, 0.1mmol), Cs2CO3 (110mg, 0.34mmol), Pd(dba)2 (5mg, 0.0085mmol) and Xanphos (4mg, 0.0085mol) in DMF(1.0mL) were degassed under N2 and then heated to 100 C for lh. After cooled, the reaction mixture was filtered. The filtrate was washed with H2O, extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated to residue, which was purified by prep-TLC (EA/PE, 1/2, v/v) to give desired compound (13mg, 52% yield). LCMS: m/z, 296.1(M+H)+; 1HNMR (400MHz, CDCl3) delta 4.24~4.44(m, 4H), 6.32~6.35(m, 1H), 6.66 (s, 1H), 6.75(d, J=8.0Hz, 1H), 7.26~7.35(m, 1H), 7.50(d, J=7.6Hz, 1H), 7.64~7.73(m, 1H), 8.62(d, J=4.8Hz, 1H).

According to the analysis of related databases, 723294-75-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HUA MEDICINE (SHANGHAI) LTD.; CHEN, Li; BALDWIN, John J.; WU, Chengde; SHEN, Chunli; WO2014/124560; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 723294-75-5, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 723294-75-5 as follows.

To a solution of 13 (50 mg, 0.2mmol) in imL of dry DMF was added 14 (53mg, 0.2mmol), C52C03 (200 mg, 0.2mmoi), Pd(dba)2 (20 mg) and Xantphos (10 mg). The mixture was degassed under vacuo and purged with N2 for several times. Then the mixture was stirred at 110C for 2h, The mixture was diluted with water (2OmL) and extracted with EtOAc (5OmL).The organic layer was washed with brine (2OmL), dried over anhydrous Na2SO4 and concentrated. The crude product was purified by prep-TLC to give the target product Compound 1 (2.8 mg, yield: 4%).LCMS: ith. 445.9(M-t-HY;1IINMR (400 MHz, CDC]3): oe857 (s, I El), .03(s, IH), ?787(s, 111), 7.82-7.83(m, IH),7 71(m IH) 7 8-7 61(m 1H) 7 54(s, 1H) 7 50-7 5(m IH) 7 47- 0 m, I H) 7 30-7 12 (m, 2H), 729-728 (m, 1H.

According to the analysis of related databases, 723294-75-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HUA MEDICINE (SHANGHAI) LTD.; CHEN, Li; LI, Yongguo; (44 pag.)WO2017/173604; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 723294-75-5 as follows. name: 3-Fluoro-5-iodobenzonitrile

A mixture of compound 1 (15mg, 0.085mmol), compound 2(25mg, 0.1mmol), Cs2CO3 (110mg, 0.34mmol), Pd(dba)2 (5mg, 0.0085mmol) and Xanphos (4mg, 0.0085mol) in DMF(1.0mL) were degassed under N2 and then heated to 100 C for lh. After cooled, the reaction mixture was filtered. The filtrate was washed with H2O, extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated to residue, which was purified by prep-TLC (EA/PE, 1/2, v/v) to give desired compound (13mg, 52% yield). LCMS: m/z, 296.1(M+H)+; 1HNMR (400MHz, CDCl3) delta 4.24~4.44(m, 4H), 6.32~6.35(m, 1H), 6.66 (s, 1H), 6.75(d, J=8.0Hz, 1H), 7.26~7.35(m, 1H), 7.50(d, J=7.6Hz, 1H), 7.64~7.73(m, 1H), 8.62(d, J=4.8Hz, 1H).

According to the analysis of related databases, 723294-75-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HUA MEDICINE (SHANGHAI) LTD.; CHEN, Li; BALDWIN, John J.; WU, Chengde; SHEN, Chunli; WO2014/124560; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 723294-75-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 723294-75-5 name is 3-Fluoro-5-iodobenzonitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Procedure for preparation of compound 2:To a solution of 13 (1000mg, 0.46mmoi) and 14 (135.8mg, 0.SSmmoi) in DMSO (2OmL) was added CuT (95mg, 0.OSmmol) and C52C03 (399.7mg, 0.92mmoi) at rt, the mixture was stirred at 100C for lOh under N2 atmosphere. The solution was diluted with EtOAc (lOmL), washedwith water, biine (iOmnL), dried over anhydrous Na2SO4, filtered and concentrated to dryness. The residue was purified by prep-TLC to afford the target product Compound 2 (5.0mg, yield:3.2 % LCMS: m/z, 338.0 ?M+H)1INNIR (400 MHz, CDCI3): .59 (d, j:::: 4.4 Hz, 111), 7.88 (d, j:::: 6.8 Hz, 1H), 759-752(m, 3H), 750-745 (m, 3H), 7.32-7.28 (m, 3H), 7.19-7.17 (m, 1H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Fluoro-5-iodobenzonitrile, and friends who are interested can also refer to it.

Reference:
Patent; HUA MEDICINE (SHANGHAI) LTD.; CHEN, Li; LI, Yongguo; (44 pag.)WO2017/173604; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com