Month: March 2021

Synthetic Route of 26670-89-3, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

2,6-Difluoro-N-(2′-methyl-5′-(pyridin-3-ylethynyl)biphenyl-4-yl)benzamide[00148] To the solution of 2-bromo-4-iodo-l-methylbenzene (0.3 g, 1.0 mmol) in TEA (4 mL) and toluene (1 mL) was added 3-ethynylpyridine (0.115 g, 1.12 mmol), CuI (0.04 g, 0.2 mmol), and Pd(PPh3)4 (0.065 g, 0.06 mmol). The resulting solution was heated at 1000C overnight before it was diluted with water and extracted with EtOAc (3chi20mL). The combined organic phases were dried and concentrated, and the column chromatography (Hexanes/EtOAc=l/l) afforded 2 in 66% yield. The desired compound was obtained from 2 through Suzuki coupling.[00149] 1H NMR (400 MHz, CDCb) delta 8.75 (d, / = 1.2 Hz, 1 H), 8.54-8.52 (m, 1 H), 7.81-7.78 (m, 1 H), 7.72-7.68 (m, 3 H), 7.45-7.43 (m, 3 H), 7.37-7.34 (m, 2 H), 7.29-7.27 (m, 2 H), 7.03 (t, / = 8.0 Hz, 2 H), 2.31 (s, 3 H); ESMS cacld (C27H18F2N2O): 424.1; found: 425.1 (M+H).

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-4-iodo-1-methylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SYNTA PHARMACEUTICALS CORP.; JIANG, Jun; ZHANG, Junyi; CHEN, Shoujun; SUN, Lijun; WO2010/39238; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 375-80-4, The chemical industry reduces the impact on the environment during synthesis 375-80-4, name is 1,6-Diiodoperfluorohexane, I believe this compound will play a more active role in future production and life.

Example 3Purification of dodecafluoro-l,6-diiodohexane (m=3) (via solution)75 mg of a commercial mixture of alpha,omega-diiodoperfluorinated compounds (sold by Apollo Scientific Ltd.) composed of 25% tetrafluoro-l,2-diiodoethane (m=l), 25% octafluoro-1,4- tetraiodobutane (m=2), 25% dodecafluoro-l,6-diiodohexane (m=3) and 25% hexadecafluoro- 1,8-diiodooctane (m=4) were solubilized in 1 ml Of CHCl3, and separately 20 mg of sequestering agent of formula (CH3^N+-(CH2)I2-N+(CH3 )3*2I~, i.e. dodecamethonium iodide, were solubilized in I mI Of CH3OH. The two solutions were then mixed in a test tube which was then closed. After about 2 hours, the formation of a solid white precipitate was observed, which was filtered, washed twice with CCU and dried under vacuum. The results of the performed tests, as reported below, confirmed that this was an adduct of dodecamethonium iodide and dodecafluoro-1,6- diiodohexane.The dodecafluoro-l,6-diiodohexane was then separated from the sequestering agent by sublimation of the crystalline adduct under vacuum at a temperature of about 500C and recovered by recondensation at a temperature of about -198C.100% pure dodecafluoro-l,6-diiodohexane was then obtained. The following tests were conducted on the crystalline adduct:- melting point: 226C;- IR (cm 1, selective bands):? pure dodecamethonium iodide: 3002, 2914, 2851, 1483, 1464, 973, 939, 916, 731;? adduct of dodecamethonium iodide and dodecafluoro-l,6-diiodohexane: 3010, 2941, 2867, 1475, 1203, 1141, 1125, 1081, 963, 909, 731.- 19F NMR (470.6 MHz, CD3OD, 0.002 M):? adduct of dodecamethonium iodide and dodecafluoro-l,6-diiodohexane:deltadelta(lComegaCF2CF2)2 = 0.08, deltadelta(lCF2CF2CF2)2 = 0.01 , deltadelta(lCF2CF2CK)2 = 0.00.An XRD test was performed on the adduct crystal which confirmed the exclusive presence of decamethonium iodide and dodecafluoro-l,6-diiodohexane. In fact, Figure 3 represents the crystalline structure of the adduct in which the molecules of dodecamethonium iodide (the carbon and nitrogen atoms are light grey coloured and the hydrogen atoms white) alternate with the molecules of dodecafluoro-l,6-diiodohexane (carbon atoms are light grey coloured, hydrogen atoms white and the iodine atoms dark grey) and with the iodide atoms (dark grey coloured). Moreover, it was observed that, at the crystalline state, decamethonium iodide and dodecafluoro-l,6-diiodohexane form alternating parallel layers, since the dodecafluoro-1,6- diiodohexane occupies the cavity defined by the spacer chain between the two nitrogen atoms of the dodecamethonium iodide and the two iodides of the same, due to the iodide-iodine interactions generated. Thus, the following crystallographic measurements are reported: As can be observed, in the adduct crystal, the difference delta (B – A) between the distance B between the iodide atoms aligned with the molecule of dodecafluoro-l,6-diiodohexane, as shown in figure 1, and the distance A between the nitrogen atoms belonging to the same dodecamethonium molecule is equal to 0.688 A and significant of the existence of said interactions I- 1~.The following tests were performed on the pure dodecafluoro-l,6-diiodohexane:- IR (cm”1, selective bands):? pure dodecafiuoro-l,6-diiodohexane: 1190, 1130, 1039, 887, 763;- 19F NMR (470.6 MHz, CD3OD, 0.002 M):? pure dodecafiuoro-l,6-diiodohexane: delta = -63.80 (ICF2CF2)2, -112.02 (ICF2CF2)2. The gas chromatography tests also confirmed that this was only 100% dodecafluoro-1,6- diiodohexane.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1,6-Diiodoperfluorohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Politecnico di Milano; WO2009/7302; (2009); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

188815-32-9, name is 3-Bromo-5-iodobenzoic acid, 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. Recommanded Product: 3-Bromo-5-iodobenzoic acid

To a solution of 3-bromo-5-iodo-benzoic acid (D7) (14.6 g, 44.7 mmol, 1 equiv) in MEOH (150 ml) at 0 C was added SOCS (3.9 ML, 53.6 mmol, 1.2 equiv). The resulting solution was refluxed for 2 h, cooled to room temperature and concentrated in vacuo. The residue was diluted with AcOEt and washed twice with 2N aqueous NAOH solution then brine, dried over MGS04 and concentrated in vacuo to give 3-bromo-5-iodo-benzoic acid methyl ester (D8a) (14.8 g, 97%) as a pale brown solid.

The synthetic route of 188815-32-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2004/50619; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, 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. Application In Synthesis of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane

General procedure: In a three-necked round flask, 9-decene-1-ol (5.0mmol) and perfluoroalkyl iodide (6.0mmol) were dissolved in a mixture of CH3CN and H2O (1:1, 10mL total). Sodium dithionate (Na2S2O4) (5.8mmol) and sodium hydrogen carbonate (NaHCO3) (5.2mmol) were added to the reaction mixture and the solution was stirred at room temperature for 4h. The reaction mixture was extracted with ethyl acetate and washed three times with water. The organic layer was dried over sodium sulfate (Na2SO4), filtered, and evaporated to yield 3a (2.433g, 96.9%) or 3b (2.786g, 92.6%) as yellow liquid.

The synthetic route of 355-43-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Miyajima, Hiroki; Kasuya, Maria Carmelita Z.; Hatanaka, Kenichi; Journal of Fluorine Chemistry; vol. 222-223; (2019); p. 24 – 30;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 6940-76-7, name is 1-Chloro-3-iodopropane, A new synthetic method of this compound is introduced below., Formula: C3H6ClI

To a suspension of NaH (22 mg, 0.85 mmol) in DMF (2.0 mL) was added S1 (305 mg, 0.78 mmol) in DMF (1.5 mL). After 10 min at room temperature, S4a (0.20 mL, 1.53 mmol) was added to this mixture, and the reaction mixture was stirred at room temperature for 6 h, diluted with ether,washed with water and dried over Na2SO4. Purification by FCC (PE/EtOAc, 8 : 1) gave the chloride S5a (344 mg, 94%) as a yellow oil.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Gao, Yan; Shan, Dong; Jia, Yanxing; Tetrahedron; vol. 70; 34; (2014); p. 5136 – 5141;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 51628-12-7, Recommanded Product: 2-(4-Iodophenyl)acetonitrile

(1) A three-necked flask was added with p-iodobenzeneacetonitrile (0.04 mol), phloroglucinol (0.02 mol) and etherAgent, zinc chloride (0.012 mol) as a catalyst, HCl gas (30 ml) was bubbled in an ice-salt bath for 1 hour to observe the reactionThe medium should change from colorless to orange. The reaction was allowed to stand in the freezer for 12 hours, and then continued to pass HCl gas (25ml)1 hour, standing in the refrigerator for 2 days, remove the reaction solution, decanting ether, water bath heated to reflux for two hours, was recrystallizedTo 2,4,6-trihydroxy-4′-iodo-phenylbenzyl ketone of general formula IIa.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Nanhua University; Zheng Xing; Zheng Qutong; Wang Zongbao; Lei Xiaoyong; Zeng Xianliang; Xiao Yan; Liu Ya; Huang Qiuxia; (23 pag.)CN106432165; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 1131614-23-7, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 1131614-23-7, name is Methyl 4-(difluoromethoxy)-3-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of methyl 4-(difluoromethoxy)-3-iodobenzoate (2 g, 6.1 mmol) from step 1 , 2-ethynylpyridine (0.94 ml_, 9.2 mmol), dichlorobistriphenylphosphine palladium(ll) (0.86 g, 1.2 mmol), copper iodide (0.23 g, 1.2 mmol) and triethylamine(1.7 ml_, 12.2 mmol) in toluene (30 ml.) was stirred at 100 0C under an atmosphere of nitrogen for six hours. After the reaction was complete, the reaction mixture was concentrated to yield a semi-solid residue. This residue was purified by flash chromatography on SiO2 (gradient elution using EtOAc/hexane 20/80) to yield the title compound as a white solid (1.47 g, 80% yield).

The chemical industry reduces the impact on the environment during synthesis Methyl 4-(difluoromethoxy)-3-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; WYETH; WO2009/143404; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

619-58-9, name is 4-Iodobenzoic acid, 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. category: iodides-buliding-blocks

248 mg (1 mmol) of 4-iodobenzoic acid and 720.54 mg (3 mmol) of sodium sulfide nonahydrate were added, copper powder 12.70 mg (0.2 mmol), ethanedithiol 8.4 uL (0.1 mmol) and 3 mL of solvent DMSO was placed in a 25 mL reaction tube equipped with a magnet, sealed with argon, heated and stirred, and reacted in an oil bath at 90 C for 12 hours. After completion of the reaction, the reaction solution was washed with NaOH solution and transferred to a 250 mL separatory funnel. The ether was extracted and the upper organic solvent was removed. The aqueous phase was adjusted to pH 1-3, extracted with dichloromethane and washed with water. Dried over magnesium sulfate. Evaporated under reduced pressure and subjected to column chromatography to afford 152 mg of product as a white solid, yield 99%

The synthetic route of 619-58-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dalian University of Technology; Liu Yajun; Xue Hongyu; Jing Bing; Liu Yong; (18 pag.)CN106916090; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 355-43-1, These common heterocyclic compound, 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, 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.

General procedure: A 25 mL of Schlenk tube equipped with a magnetic stir bar were charged with aniline (1.2 mmol, 3.0 equiv), K2CO3 (0.8 mmol, 2.0 equiv) and fac-Ir(ppy)3 (0.26 mg, 0.0004 mmol, 0.1 mol %) under air. The vessel was evacuated and backfilled with Ar (3 times), CnF2n+1I (n=6, 4, 2; 0.4 mmol, 1.0 equiv), anhydrous 1,2-dichloroethane (4 mL) were then added. The tube was screw capped and stirred at room temperature under irradiation of blue LEDs (12 W) for 24 hours. The reaction mixture was filtered through a pad of Celite and washed with ethyl acetate (3¡Á5 mL). The filtrate was concentrated. The residue was subjected to column chromatography on silica gel to afford the pure product.

The synthetic route of 355-43-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; He, Chun-Yang; Gu, Ji-Wei; Zhang, Xingang; Tetrahedron Letters; vol. 58; 41; (2017); p. 3939 – 3941;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. HPLC of Formula: C6H3ClINO2

The appropriate product 2 (1 mmol, 1 eq) in AcOH/EtOH (1:1, 0.42 M) was added slowly to a solution of Iron powder (6 eq) in AcOH/EtOH(1:2, 2 M) at 60C . The solution was stirred at 70C for 30-60 mins. The reaction mixture was cooled to 23C , filtered through celite, washed with ethyl acetate, and concentrated. The oily residue was dissolved in ethyl acetate (30 mL), washed with saturated aq. NaHCO3 (1 x 15 mL), water (2 x 10 mL), dried (MgSO4) and concentrated. The oily residue was used without further purification.

The synthetic route of 1-Chloro-2-iodo-4-nitrobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Fangying; Jiang, Hongxia; Deng, Yufang; Yu, Jiang; Zhan, Miao; Zhao, Lifeng; Chen, Yuanwei; Bioorganic and Medicinal Chemistry Letters; vol. 28; 14; (2018); p. 2399 – 2402;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com