Tag: M.W=400-500

Reference of 355-43-1, 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 355-43-1 as follows.

General procedure: To a 25 mL of Schlenk tube equipped with a Teflon septum were added Ru(bpy)3Cl2 (1.5 mg, 0.5 mol%), Cs2CO3 (130 mg, 1.0 equiv) and 1 (0.4 mmol, 1.0 equiv) followed by DMSO 3.0 mL) with stirring. Perfluoroalkyl iodine (2.0 equiv.) was then added subsequently under Ar. The Schlenk tube was screw capped and the reaction was then under irradiated with a 12 W blue LEDs (460 nm-470 nm). After stirring for 24 h, the reaction mixture was diluted with ethyl acetate, washed with brine, the organic phases were collected and dried over anhydrous Na2SO4, filtered and concentrated. The residue was purified with silica gel chromatography to provide pure product.

According to the analysis of related databases, 355-43-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Ben-Hou; Kong, Jing-Jing; Huang, Yang; Lou, Yue-Guang; Li, Xiao-Fei; He, Chun-Yang; Chinese Chemical Letters; vol. 28; 8; (2017); p. 1751 – 1754;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 626-44-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 626-44-8, name is 1,3,5-Triiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 3 (98.0 mg, 0.211 mmol), 4 (0.06 mL, 0.42 mmol), PdCl2(PPh3)2 (14.8 mg, 0.021 mmol), PPh3 (11.1 mg, 0.042 mmol), CuI (4.0 mg, 0.021 mmol), Et3N (4.0 mL), and THF (5.0 mL) was placed in a round-bottom flask equipped with a magnetic stirring bar. After degassing the reaction mixture several times, the reaction was carried out at 40 ¡ãC for 3 h with stirring. After the reaction mixture was cooled to room temperature, CHCl3 was added to the mixture. The mixture was filtered by Celite, and the solvent was evaporated. The residue was subjected to SiO2 column chromatography (hexane as an eluent) to obtain 6 (30.6 mg, 0.067 mmol, 32percent), S1 (40.2 mg, 0.088 mmol, 42percent), and 5 (4.0 mg, 0.086 mmol, 4percent) as colorless solids.

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, 1,3,5-Triiodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Morisaki, Yasuhiro; Gon, Masayuki; Tsuji, Yuichi; Kajiwara, Yuichi; Chujo, Yoshiki; Tetrahedron Letters; vol. 52; 42; (2011); p. 5504 – 5507;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, molecular formula is C6F13I, 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. Safety of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane

A Schlenk flask was charged with alkoxy ester 10b (3.48g, 10.0mmol), copper powder (1.40g, 22.0mmol), 2,2?-bipyridyl (20mg, 0.13mmol), DMSO (40mL) and hexafluorobenzene (80mL). The mixture was heated to 70C and perfluorohexyl iodide (4.47g, 22.0mmol), dissolved in hexafluorobenzene (20mL), was dropwise added. The mixture was then heated to 105C for 72h. After cooling to r.t., the mixture was partitioned between water (60mL) and dichloromethane (60mL) and the heterogeneous mixture formed was filtered over short silica gel column. The organic layer was separated and the aqueous layer was extracted with dichloromethane (3¡Á60mL). The combined organic layers were dried with anhydrous magnesium sulfate, the drying agent was filtered off and the solvent was removed on a rotary vacuum evaporator (40C, 1h, 25kPa) to give the target ester 11b (5.19g, 95.9%, colourless viscous oil).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 355-43-1, its application will become more common.

Reference:
Article; Kvi?ala, Jaroslav; Schindler, Martin; Kelbichova, Vendula; Babun?k, Mario; Ryba?kova, Marketa; Kvi?alova, Magdalena; Cva?ka, Josef; B?ezinova, Anna; Journal of Fluorine Chemistry; vol. 153; (2013); p. 12 – 25;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 626-44-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 626-44-8, name is 1,3,5-Triiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a mixture of 3-methoxy-6-(trimethylsilyl)ethynylpyridazine(0.185 g, 0.766 mmol), 1,3,5-triiodobenzene (0.100 g, 0.219 mmol), Pd2(dba)3(0.020 g, 0.021 mmol), CuI (0.004 g, 0.021 mmol), PPh3 (0.005 g, 0.021 mmol) under nitrogen atmosphere were added dry Et3N (10 mL) and toluene (10 mL). The reaction mixture was cooled to 0 C and TBAF (1 M in THF, 1.53 mL) was added dropwise and the reaction mixture was stirred for 10 min. The solution was heated to50C for 48 h. The reaction was cooled,filtered through Celiteandevaporated under reduced pressure. The crude product was purified by column chromatography on silica gel (petroleum ether/ethyl acetate2:1) to give the title compound1as a brown solid (0.055 g, 55percent).

The synthetic route of 1,3,5-Triiodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Martin, Flavia-Adina; Baudequin, Christine; Fiol-Petit, Catherine; Darabantu, Mircea; Ramondenc, Yvan; Ple?, Nelly; Tetrahedron; vol. 70; 15; (2014); p. 2546 – 2555;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 355-43-1, 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 355-43-1 as follows.

In a 25 mL round bottomed flask, was placed under N2 atmosphere a mixture of 2 (0.66 g, 2.0 mmol), perfluoro 1-iodohexane or perfluoro 1-iodooctane (2.5 mmol), AIBN (13 mg, 0.08 mmol) and 2 mL of 1,2-dichloroethane. The mixture was then stirred at 75C for 18 h. After cooling to room temperature, the solvent was removed under vacuum and the residue was subjected to a column chromatography on silica gel (ethyl acetate/hexane: 1/3) followed by a recrystallization in ethanol, to provide 3a and 3b as white solids. 4.3.1. 4′-{(4,4,5,5,6,6,7,7,8,8,9,9,9-tridecafluoro-2-iodononyl)oxy}-(1,1′-biphenyl)-4-yl benzoate (3a) Yield: 89%. 1H NMR (CDCl3) d 8.25 (d, 2H, J = 7.5 Hz), 7.5-7.7 (m,7H), 7.30 (d, 2H, J = 8.2 Hz), 7.0 (d, 2H, J = 8.5 Hz), 4.55 (quint., 1H, CHI), 4.21-4.38 (dd, 2H,2J = 10.5 Hz,3J = 4.8 Hz, CHICH2O), 2.85-3.23 (m, 2H, CF2CH2CHI). 13C NMR (CDCl3) d(ppm) 165.2(CO), 157.2 (ArO), 150.1 (ArO), 138.3, 134.2, 133.6, 130.2, 129.51, 128.5, 128.3, 127.8, 121.9, 115.2, 72.8 (CH2O), 37.8 (t,2JCF= 21 Hz, CF2CH2), 12.7 (CI). 19F NMR (CDCl3) d(ppm) 80.5 (t, CF3, 3JFF= 10.0 Hz), 113.1 & 113.3 (dm & dm, 21F, JA-B= 295 Hz, 2 diastereoisomers of CHICH2CF2), 121.5 (m, 2F), 122.6 (m,2F), 123.3 (m, 2F), 125.8 (m, 2F). HRMS (ESI) calculated for C28H18F13IO3Na+: 799.314 (found: 799.005).

According to the analysis of related databases, 355-43-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Marzouk, Samir; Khalfallah, Ali; Heinrich, Benoit; Khiari, Jamel Eddine; Kriaa, Abdelkader; Mery, Stephane; Journal of Fluorine Chemistry; vol. 197; (2017); p. 15 – 23;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, 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 63262-06-6, HPLC of Formula: C6H2Br2I2

To a 100 ml Schlenk reaction vessel were added under a nitrogen atmosphere 4.39 g (9.00 mmol) of 1,4-dibromo-2,5-diiodobenzene (compound of the formula (5)) synthesized in Synthetic Example 1, 974 mg (0.84 mmol) of tetrakis(triphenylphosphine)palladium (manufactured by Tokyo Chemical Industry Co. Ltd.) as a catalyst, and 4.16 g (20.7 mmol) of 2-bromophenylboronic acid (manufactured by Sigma-Aldrich) (compound of the formulae (6) and (7)). Further, 72 ml of toluene, 18 ml of ethanol, and an aqueous solution composed of 5.72 g (54.0 mmol) of sodium carbonate and 22 ml of water were added. The whole was immersed in an oil bath at 85C and stirred for 15 hours. After cooling to room temperature, dichloromethane and a saturated aqueous sodium chloride solution were added and phase separation was conducted. The organic phase was concentrated under reduced pressure. The residue was recrystallized from toluene to obtain white needle-like crystals (3.68 g, yield 75%). Melting point: 230-231C. 1H-NMR (CDCl3, 21C): delta=7.70 (d, J=8.0Hz, 2H), 7.55 (d, J=1.5Hz, 2H), 7.45-7.23 (m, 6H). MS m/z: 546 (M+, 92%), 466 (M+-Br, 45), 386 (M+-2Br, 53), 226 (M+-4Br, 100).

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; Tosoh Corporation; EP2067782; (2009); 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. Formula: C6F13I

Cooled to -78 C. zirconocene dichloride(Cp 2 ZrCl 2, 70.2 mg, 0.24 mmol)Of ether (2.4 mL)To the solution was added n-propylmagnesium chloride (2.0 M in ether solution, 0.12 mL, 0.24 mmol)1,4-Dioxane (23 [mu] L, 0.27 mmol)And n-tridecafluorohexyl iodide (C 6 F 13 I, 78 muL, 0.36 mmol) were added,And the mixture was stirred at the same temperature for 1 hour.Then,Methylaluminoxane(10% toluene solution, 0.16 mL, 0.24 mmol) was added thereto, the temperature was raised to 0 C., and the mixture was stirred for 2 minutes. After adding styrene oxide (23 muL, 0.20 mmol) to this, the temperature was raised to room temperature and stirred for 1 hour.After completion of the reaction, 1 N hydrochloric acid was added to quench the reaction and then extracted 3 times with ether, and the organic layers were combinedDried over sodium sulfate, filtered and the solvent was distilled off under reduced pressure to give a crude product. The crude product obtainedThe product was purified by silica gel column chromatography (hexane / ethyl acetate = 20/1 (v / v)) To obtain 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecaFluoro-1-phenyl-2-hydroxyoctane (77.5 mg, yield: 88%).

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

Reference:
Patent; TOKYO INSTITUTE OF TECHNOLOGY; TOSOH F-TECH INCORPORATED; MIKAMI, KOICHI; FUJIU, MOTOHIRO; (46 pag.)JP5894739; (2016); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 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, it is a common compound, a new synthetic route is introduced below. name: 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane

General procedure: In a Pyrex glass tube were placed TTMSS (0.2 mmol), olefin (0.24 mmol), perfluoroalkyl iodide (0.24 mmol) and CH2Cl2 (5 mL). Then Na2S2O3 (0.5 mmol, 79 mg) and water (1 mL) were added to the mixture. After sealing the tube, the mixture was shaken and then irradiated with a Hg lamp at room temperature. After the reaction was completed, the mixture was extracted with CH2Cl2. The extract was washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to afford pure product. 4.2.4 Ethyl 2-methyl-3-perfluorohexylpropanoate (6a) Colorless oil. 1H NMR (400 MHz, CDCl3) delta 4.20 (q, J = 7.2 Hz, 2H), 2.90 (m, 1H), 2.73 (m, 1H), 2.09 (m, 1H), 1.30 (d, J = 7.6 Hz, 3H), 1.25 (t, J = 7.2 Hz, 3H); 13C NMR (150 MHz, CDCl3) delta 174.6, 61.1, 34.9 (t, JC-F = 21.1 Hz, C6F13C), 32.8, 18.3, 14.0; IR (KBr) 2962, 1735, 1240, 1219, 1146, 806, 697 cm-1; HRMS (ESI+) m/z calcd for C12H11F13O2Na [M+Na]+ 457.0450, found 457.0444.

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

Reference:
Article; Yajima, Tomoko; Yamaguchi, Kanako; Hirokane, Rie; Nogami, Emiko; Journal of Fluorine Chemistry; vol. 150; (2013); p. 1 – 7;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

63262-06-6,Some common heterocyclic compound, 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, molecular formula is C6H2Br2I2, 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.

To an oven dried round bottom flask was added 1 (14.5 g, 29.8 mmol) and (0206) tetrakistriphenylphosphinepalladium(O) (1.7 g, 1.5 mmol) before a 0.5 M (3-bromothiophen- 2-yl)zinc(ll) bromide solution in THF (125 ml_, 62.5 mmol) was added. The reaction mixture was stirred and heated at 65 C (oil bath temperature) overnight. The mixture was cooled to room temperature and poured into 150 ml_ of saturated aqueous ammonium chloride solution. The precipitate was filtered off and washed with water, acetone and diethyl ether. Compound 2 was recovered as an off-white solid (1 1.6 g, 20.8 mmol, 70% yield). 1 H NMR (400 MHz, CDCIs): delta 7.74 (s, 2H), 7.44 (d, J = 5.3 Hz, 2H), 7.1 1 (d, J = 5.3 Hz, 2H). 13C NMR (100 MHz, CDCI3): delta 136.63, 136.11 , 135.17, 130.51 , 126.97, 123.53, 1 11.79, 77.16. HRMS (El): m/z calcd for Ci4H6Br4S2 (M+) 557.6603 found 557.6603.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,4-Dibromo-2,5-diiodobenzene, its application will become more common.

Reference:
Patent; IMPERIAL INNOVATIONS LIMITED; WADSWORTH, Andrew; NIELSEN, Christian; HOLLIDAY, Sarah; MCCULLOCH, Iain; KNALL, Astrid-Caroline; PURUSHOTHAMAN, Balaji; (81 pag.)WO2017/191468; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

63262-06-6, These common heterocyclic compound, 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, 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.

Under an argon atmosphere, dibromodiiodobenzene (4.00 g, 8.20 mmol), compound 1-2 (6.81 g, 16.8 mmol, 1.05 eq.), and Pd(PPh3)4 (474 mg, 0.41 mmol, 5% Pd) were dissolved in 1 ,2-dimethoxyethane (800 mE) and water (200 mE) in which K3P04 (10.4 g, 49.2 mmol) was dissolved was added thereto, and the mixture was stirred with heating at 500 C. for 24 hours. Afier completion of the reaction, extraction with ethyl acetate was conducted, and the solvent was concentrated. The resulting solid was purified by column chromatography, whereby obtaining a white solid (5.0 g, yield: 77%). The obtained solid was compound 1-3, which is an intended product, and by mass spectrum analysis, it was confirmed that it had an mle value of 790 with respect to a molecular weight of 790.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 63262-06-6.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; Takahashi, Ryota; Ikeda, Hidetsugu; Seda, Keita; Nakano, Yuki; (152 pag.)US10249832; (2019); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com