Tag: M.W=400-500

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,
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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,
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Related Products of 355-43-1, 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. 355-43-1 name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, 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.

In a three-necked flask (200 mL) equipped with a condenser tube, 8.93 g (20.0 mmol) of perfluorohexyl iodide, 1.70 g (10.0 mmol) of 10-undecenol, 0.657 g of azobisisobutyronitrile (4.00 mmol), and the interior of the vessel was purged with argon and then heated at 80 C. for 8 hours with stirring. The reaction mixture was dissolved in 100 ml of ethanol and 5.00 g (76.5 mmol) of zinc powder was added and stirred for 15 minutes, then 3.00 g (50.0 mmol) of acetic acid was added and the mixture was heated under reflux for 5 hours. After cooling to room temperature, it was filtered through celite to remove residual zinc powder. After concentrating the filtrate under reduced pressure, diethyl ether was added and washed with water to remove excess acetic acid. After concentration under reduced pressure, recrystallization in hexane gave 4.04 g (yield 82%) of fluorinated alcohol (III-1) C 6 F 13 – (CH 2) 11 -OH.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, and friends who are interested can also refer to it.

Reference:
Patent; NEOS Corporation; Morioka, Kyoichi; Miyata, Koji; Terauchi, Shunji; Narimatsu, Shinsuke; Umeda, Takahiko; (14 pag.)JP6091963; (2017); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 2043-57-4, A common heterocyclic compound, 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, molecular formula is C8H4F13I, 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.

(W) Synthesis of 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium 1,1,2,2-tetrafluoroethanesulfonate; 1-Methylimidazole (4.32 g, 0.52 mol) was partially dissolved in reagent-grade toluene (50 ml) in a large round-bottomed flask and stirred vigorously. 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane (26 g, 0.053 mol) was added, and the mixture was heated under reflux at 110 degrees C. for 24 hours. The solvent was removed under vacuum giving 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide (30.5 g) as a waxy solid. Potassium 1,1,2,2-tetrafluoroethanesulfonate (TFES-K, 12 g) was added to reagent grade acetone (100 ml) in a separate round-bottomed flask, and this solution was carefully added to the 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide which had been dissolved in acetone (50 ml). The reaction mixture was heated under reflux for approximately 16 hours. The reaction mixture was then filtered using a large frit glass funnel to remove the white Kl precipitate formed, and the filtrate was placed on a rotary evaporator for 4 hours to remove the acetone. The oily liquid was then filtered a second time to yield the product, as shown by proton NMR.

The synthetic route of 2043-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Harmer, Mark Andrew; Junk, Christopher P.; Vickery, Jemma; Miller, Robert; US2007/66852; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 88-82-4, 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. 88-82-4, name is 2,3,5-Triiodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 25 3,5-Diiodobenzyl-n-Hexyl Carbonate Preparation of s in Table I: Using the procedure of B, Gaux and D. LeHenaff, Bull. Soc. Chem. Fr., 34, 505 (1974), 2,3,5-triiodobenzoic acid (Aldrich) was treated with lithium aluminum hydride to give 3,5-diiodobenzyl alcohol with m.p. of 136.5-140 (literature 137).

The synthetic route of 2,3,5-Triiodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lafayette Pharmacal Inc.; US4175544; (1979); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 2043-57-4, 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 2043-57-4 as follows.

General procedure: Under an argon atmosphere, fluorinated iodide (11-13) (1.19 mmol, 1 equiv) and NaN3 (3.57 mmol, 3equiv) were dissolved in DMF (7.2 mL). Stirring was continued for 3-3.5h at 65 C. Then, solvent was evaporated under reduced pressure and reaction mixture was poured into H2O (10 mL) and extracted with Et2O (3 x 10 mL). The combined organic layers were washed with brine (2 x 10 mL) and dried over Na2SO4. The solvent was removed under vacuum to afford 9, 16, 17.

According to the analysis of related databases, 2043-57-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Tomaszewska, Joanna; Koroniak-Szejn, Katarzyna; Koroniak, Henryk; Arkivoc; vol. 2017; 2; (2016); p. 421 – 432;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 626-44-8,Some common heterocyclic compound, 626-44-8, name is 1,3,5-Triiodobenzene, molecular formula is C6H3I3, 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.

A mixture of 1,3,5-triiodobenzene (0.46 g, 1.0 mmol), diphenylphosphine oxide (0.73 g, 3.6 mmol), CuI (0.06 g, 0.30 mmol), l-proline (0.04 g, 0.30 mmol), and Cs2CO3 (1.5 g, 4.5 mmol) was added to toluene solution (30 mL). The mixture was refluxed under nitrogen for 48 h. After the reaction finished, the reaction mixture was extracted with dichloromethane and washed with water. The organic layer was dried by anhydrous MgSO4 and filtered. The product was isolated by silica gel column chromatography using methanol/ethyl acetate (1:5) as eluent to afford a white solid (0.64, 52%). 1H NMR (300 MHz, CDCl3, delta): 8.08 (t, J = 11.9 Hz, 3H), 7.52 (dd, J = 12.9, 7.2 Hz, 18H), 7.39 (dd, J = 9.8, 4.8 Hz, 12H). 13C NMR (75 MHz, CDCl3, delta): 141.05, 141.02, 140.91, 134.89, 134.66, 134.39, 133.00, 131.36, 131.19, 31P NMR (121 MHz, CDCl3, delta): 27.59. HRMS [m/z]: calcd for C42H33O3P3, 678.1643; found, 679.1711 [M+H+]. Anal. Calcd. for C42H33O3P3: C, 74.33; H, 4.90. Found: C, 74.36; H, 4.88.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3,5-Triiodobenzene, its application will become more common.

Reference:
Article; Ban, Xinxin; Sun, Kaiyong; Sun, Yueming; Huang, Bin; Jiang, Wei; Organic electronics; vol. 33; (2016); p. 9 – 14;,
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: In a Pyrex glass tube were placed olefin (0.2 mmol), perfluoroalkyl iodide (1.0 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 shaked 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.

Statistics shows that 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane is playing an increasingly important role. we look forward to future research findings about 355-43-1.

Reference:
Article; Yajima, Tomoko; Jahan, Ishrat; Tonoi, Takayuki; Shinmen, Manami; Nishikawa, Aya; Yamaguchi, Kanako; Sekine, Izumi; Nagano, Hajime; Tetrahedron; vol. 68; 34; (2012); p. 6856 – 6861;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, 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: 2043-57-4

The catalyst of Preparation Example 6 (15 g) was placed in a stainless-steel reaction tube having an inside diameter of 10 mm and length of 250 mm, and was heated to 180 C. with a heater. CF3CF2 (CF2CF2)2CH2CH2I and water were introduced into a vaporizer at a rate of 2.5 g/hr and 12 g/hr, respectively, and were vaporized. Air was introduced into the reaction tube as a carrier gas at a rate of 35 cc/min. The vaporized gases were carried to the catalyst in the above reaction tube by the air to cause a catalytic reaction on the catalyst. Reaction products were recovered with an ice trap and a dry ice/methanol trap provided at the outlet of the reaction tube. The GC analysis of the products revealed that an alcohol was formed at the degree of conversion of 93% and selectivity of 95%.

The synthetic route of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daikin Industries, Ltd.; US6664430; (2003); B1;,
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. 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C6H2Br2I2

Add to a 300mL Schlenk tube with argon replacement equipped with a stir bar1,4-dibromo-2,5-diiodobenzene (25.0g, 51mmol), phenylboronic acid (13.1g, 107mmol), tetrakis(triphenylphosphine) palladium (8.95g, 7.7mmol), toluene (200mL) ,Water (80mL) and potassium carbonate (35.7g, 258mmol), after sealing,Stir at 100C for 16 hours. Then, the reaction vessel was allowed to cool for 4 hours to near room temperature, and the precipitate was collected by filtration. Then, wash with water and methanol,Thus, the target compound (A1) is obtained(The yield is 15.6 g, the yield is 78.4%).

The synthetic route of 63262-06-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guandong Chemical Co., Ltd.; Xi Weitaiyi; Ji Guangdayou; Zuo Tenghuixing; Yan Jingxin; Xin Neicongchang; (45 pag.)CN111253264; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com