Tag: M.W=400-500

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 626-44-8 as follows. Recommanded Product: 1,3,5-Triiodobenzene

Synthesis of 1 , 3 , 5-tris [( 1 , 3-diethylcarboxylate-5- ( 4- (ethynyl ) phenyl )) butadiynyl ] -benzene (compound 6). 1,3,5- Triiodobenzene (5, 1.1 g, 2.41 mmol), compound 4 (3.0 g, 11.1 mmol), THF (100 ml), and diisopropylamine (50 ml) are combined in a 500 mL Schlenk flask equipped with a magnetic stir bar and a rubber stopper. The mixture is cooled to -78 °C in an acetone/dry ice bath and subjected to three cycles of brief vacuum-degas/N2 back-fill with no stirring. Then Pd(PPh3)4 (450 mg, 0.39 mmol) and Cul (150 mg, 0.79 mmol) is added to this degassed solution under positive N2 flow and the mixture is degassed for three more cycles. The solution is stirred for 48 h at 25 °C, concentrated, and dried under high vacuum. The remaining brown paste is redissolved in a minimum amount of CHCI3, and column chromatographed over silica gel using CHCI3 (stabilized with 2percent ethanol) to give a brown solid (2.1 g) , which is recrystallized three times from CHCl3:EtOH (75 ml, 2:1, v/v) to give the product 6 as an off-white solid. Yield = 1.7 g (80percent). XH NMR (500 MHz, CDC13) is shown in Fig. 16, where delta 1.42 (t, J = 7.0 Hz, 18H, -C02CH2C) , 4.43 (q, J = 7.0 Hz, 12H, -C02Cfi2CH3) , 7.65 (s, 3H, Ar2-fi) , 8.35 (d, J = 1.5 Hz, 6H, Ari-H) , 8.67 (t, J = 1.5 Hz, 3H, Ari-H) . 13C NMR (126 MHz, CDCI3) is shown in Fig. 17, where delta 14.43, 61.88, 75.13, 75.50, 79.78, 80.63, 122.45, 123.00, 131.29, 131.60, 136.72, 137.36, and 164.92.

According to the analysis of related databases, 626-44-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NORTHWESTERN UNIVERSITY; FARHA, Omar, K.; HUPP, Joseph, T.; WILMER, Christopher, E.; ERYAZICI, Ibrahim; SNURR, Randal, Q.; GOMEZ-GUALDRON, Diego, A.; BORAH, Bhaskarjyoti; WO2013/192146; (2013); A1;,
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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. 626-44-8, name is 1,3,5-Triiodobenzene, A new synthetic method of this compound is introduced below., Formula: C6H3I3

A solution of 1,3,5-triiodobenzene (0.226 g, 0.497 mmol),2-ethynyl-4,6-dimethylpyrimidine (0.229 g, 1.739 mmol),Pd(PPh3)2Cl2(0.034 g, 0.049 mmol), CuI (0.018 g, 0.097 mmol) inEt3N (15 mL) was stirred at 90C for 24 h under nitrogen atmosphere, the TLC monitoring indicated the consumption of startingmaterials. The reaction mixture was cooled,filtered through Celiteand evaporated under reduced pressure. The crude product waspurified by column chromatography on silica gel (EtOH was usedfor thefirst purification followed by a second one with ethyl acetateas eluent) to afford the title compound3as brown solid (0.097 g,42percent). Mp: 230C. IR (cm1, neat): 2962, 2923, 2900, 2172, 1949,1738, 1587, 1535, 1441, 1346, 1251, 1176, 1036, 956, 943, 845, 788,761, 704, 634, 619;1H NMR (300 MHz, CDCl3)d(ppm): 2.52 (s, 18H),7.01 (s, 3H), 7.88 (s, 3H);13C NMR (75 MHz, CDCl3)d(ppm): 24.0,84.3, 89.4, 119.5, 122.8, 136.6, 152.2, 167.3; HRMS: calcd forC30H25N6[MH]469.2141; found 469.2144.

The synthetic route of 626-44-8 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;,
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Related Products of 2043-57-4, 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.

The entire procedure including the isolation and characterization of the product was performed under an inert atmosphere (N2). n-BuLi (0.94 mL, 2.4 mmol, 1.0 equiv, 2.5 mol/L solution in hexane) was added at r.t. to a solution of Ph2PH (438 mg, 2.40 mmol, 1.0 equiv) in abs THF (2 mL). After stirring the mixture for 5 min at 23 C, perfluorinated iodide 19 (1.12 g, 2.40 mmol, 1.0 equiv) was added and the mixture was further stirred for 17 h at 23 C. The mixture was then filtered using a reversible frit and the resulting solution was evaporated to furnish the product 20 (1.11 g, 2.09 mmol, 89%) as an off-white solid; mp 40 C. IR (ATR): 3072 (w), 1482 (w), 1439 (w), 1364 (w), 1235 (m), 1182 (s), 1139 (s), 1121 (m), 1070 (m), 1028 (w), 925 (w), 847 (w), 746 (m), 735 (m), 723 (m), 693 cm-1 (s). 1H NMR (300 MHz, CDCl3): delta = 2.05-2.23 (m, 2 H), 2.24-2.37 (m, 2 H), 7.33-7.41 (m, 6 H), 7.42-7.51 (m, 4 H). 31P{1H} NMR (203 MHz, CDCl3): delta = -16.05 (s). The 13C NMR spectrum was in accordance with literature data. HRMS (ESI): m/z [M + Na]+ calcd for C20H14F13NaP: 555.0523; found: 555.0529.

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

Reference:
Article; Alpers, Torben; Muesmann, Thomas W. T.; Temme, Oliver; Christoffers, Jens; Synthesis; vol. 50; 17; (2018); p. 3531 – 3539;,
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Synthetic Route of 355-43-1, 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. 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, This compound has unique chemical properties. The synthetic route is 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.

The chemical industry reduces the impact on the environment during synthesis 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane. I believe this compound will play a more active role in future production and life.

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;,
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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. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, A new synthetic method of this compound is introduced below., Recommanded Product: 2043-57-4

1/T,liy,2No.,2No.-Perfluorooctyl thiouronium iodide (5); In a 100 mL round bottomed flask, thiourea (1.13g, 14.8 mmol) was added to a stirred solution of lH,lH,2H,2H-perfluorooctyl iodide (3.62 mL, 14.8 mmol) in ethyl alcohol (14.0 mL). The mixture was left to reflux at 78C for 13 hours under a nitrogen atmosphere then cooled to room temperature. The solvent was removed under reduced pressure to reveal a cream/white solid (8.10 g, 14.7 mmol, quantitative yield). This was used in the next step without further purification.

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

Reference:
Patent; ISIS INNOVATION LIMITED; GOUVERNEUR, Veronique; BEJOT, Romain; WO2010/7363; (2010); A2;,
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Synthetic Route of 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.

Under an argon atmosphere, dibromodiiodobenzene (2.5 g, 5.1 mmol), Intermediate 3 (4.97 g, 15.4 mmol), and Pd(PPh3)4 (237 mg, 0.205 mmol) were dissolved in toluene (250 mE) and dimethylsulfoxide (DMSO, 50 mE), 2 MNa2CO3 aqueous solution (13 mE) was added thereto, and the mixture was stirred with heating at 90 C. for 24 hours. Afier completion of the reaction, toluene was removed under reduced pressure, and the precipitated solid was filtered off. This solid was washed with methanol and ethyl acetate,whereby obtaining a white solid (2.5 g, yield: 75%). The obtained solid was Intermediate 4, which is an intended product, and by mass spectrum analysis, it was confirmed that it had an mle value of 626 with respect to a molecular weight of 626.

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

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; Takahashi, Ryota; Ikeda, Hidetsugu; Seda, Keita; Nakano, Yuki; (152 pag.)US10249832; (2019); B1;,
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Electric Literature of 355-43-1,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.

1.Tetramethyl hydrazine (1.0 mmol) was placed in a 25 mL round bottom flask at room temperature.2 mL of acetonitrile (water content 0.1%) solvent was injected, and then perfluoroiodohexane (1.1 eq) was added.The reaction was carried out under 36 W CFL light, and TLC was monitored until the reaction was complete (about 10 h).The obtained reaction product was poured into 100 mL of water, extracted three times with dichloromethane, and the organic phase was dried, and the organic solvent was evaporated under reduced pressure to give a crude product; 2.The crude product was subjected to silica gel column chromatography (silica gel needs to be pretreated with Et3N/PE=1:9 overnight), and eluted with an eluent (petroleum ether: ethyl acetate = 1:1 (V:V)). Eluent, distillation under reduced pressure,Obtained a white solid,It is the product N-[bis(dimethylamino)methylidene]-2,2,3,3,4,4,5,5,6,6,6-undecafluorohexanamide,The yield is 79%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, its application will become more common.

Reference:
Patent; Liaoning University; Liang Fushun; Wang Rui; Su Zhongmin; (13 pag.)CN109369467; (2019); A;,
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. 626-44-8, name is 1,3,5-Triiodobenzene, A new synthetic method of this compound is introduced below., Computed Properties of C6H3I3

1,3,5-triiodobenzene (33.0 g, 0.10 mol), Pd(dppf)Cl2.CH2Cl2 (700 mg, 0.86 mmol) under nitrogen atmosphereCuI (330 mg, 1.73 mmol) and isopropylamine (60 ml) were added to tetrahydrofuran (400 ml), and stirred at room temperature for 10 min.Trimethylsilylacetylene (32.3 g, 0.33 mol) was slowly added by syringe, and the mixture was warmed to 80 ° C and stirred for 12 hours.TLC showed the end of the reaction, and a silica gel column (PE/EA = 4/1 to 2/1) gave Compound 11 (33.0 g, yield 90percent).

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:
Patent; Shanghai Hehui Optoelectric Co., Ltd.; Wu Fan; (24 pag.)CN108530431; (2018); A;,
Iodide – Wikipedia,
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Application 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: 2-(Perfluorodecyl)ethyl iodide (5.26 g, 7.81 mmol), 4-mercaptophenol (0.94 g, 7.44 mmol), andK2CO3 (2.06 g, 14.88 mmol) was added in acetone (80 mL) in a 200 mL recovery flask, and theresulting mixture was heated at reflux for 3 days. The reaction mixture was allowed to cool toroom temperature. After 1 N HCl aqueous solution was added to the mixture until pH ? 3,saturated NaCl aqueous solution (100 mL) was added to it and the resulting solution wasextracted with EtOAc (100 mL × 3). The organic layers were combined and dried with MgSO4,and after filtration, the filtrate was concentrated using a rotary evaporator under reduced pressure.The crude product was purified by silica gel column chromatography (eluent: CHCl3) to give A-10 (3.00 g, 4.46 mmol) in 60% yield as colorless powder.

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; Yoshida, Tomohiro; Hirakawa, Tomomi; Nakamura, Toru; Yamada, Yasuhiro; Tatsuno, Hiroko; Hirai, Masayuki; Morita, Yuki; Okamoto, Hiroaki; Bulletin of the Chemical Society of Japan; vol. 88; 10; (2015); p. 1447 – 1452;,
Iodide – Wikipedia,
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Application of 63262-06-6, 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 63262-06-6 as follows.

Under a nitrogen atmosphere,4.00 g (33.2 mmol) of 2,2,6,6-tetramethylpiperidine (Wako Pure Chemical Industries) and 12 ml of THF (dehydrated grade) were added to a 300 ml Schlenk reaction vessel.At 0 C.,Isopropyl magnesium chloride33.0 ml (42.9 mmol) of lithium chloride (Sigma-Aldrich, 1.3 M) in THF solution was added,And the mixture was stirred at room temperature for 2 days.The resulting magnesium chloride 2,2,6,6-tetramethylpiperidide5.18 g (45.3 mmol) of 3-methoxythiophene (Wako Pure Chemical Industries) was added dropwise to the lithium chloride solution,And aged at room temperature for 8 hours.20 ml of THF (dehydration grade) was added,It was cooled to -60 C.Here,A solution consisting of 6.13 g (45.0 mmol) of zinc chloride (Wako Pure Chemical Industries) and 40 ml of THF (dehydration grade) was charged using a Teflon cannula.Further washing was carried out using 10 ml of THF (dewatering grade).After gradually raising the temperature to room temperature,To the obtained white slurry liquid (3-methoxythienyl-2-zinc chloride)7.01 g (14.4 mmol) of 1,4-dibromo-2,5-diiodobenzene (Tokyo Chemical Industry Co., Ltd.)244 mg (0.214 mmol, 1.49 mol% based on 1,4-dibromo-2,5-diiodobenzene) of tetrakis (triphenylphosphine) palladium (Tokyo Chemical Industry)The obtained mixture was reacted at 50 C. for 8 hours.After cooling to room temperature,The whole was concentrated under reduced pressure.To the resulting residue were added 100 ml of water and 100 ml of hexane and filtered.The solid obtained by filtration was purified by silica gel column chromatography (hexane / toluene = 2/1 to 0/1) and recrystallized from toluene to give 1,4-di (3-methoxythienyl) -2, 4.19 g of 5-dibromobenzene as a pale yellow solid (yield 63%).

According to the analysis of related databases, 63262-06-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TOSOH CORPORATION; WATANABE, MAKOTO; UENO, WATARU; UEDA, SAORI; HACHIYA, HITOSHI; (12 pag.)JP2017/31098; (2017); A;,
Iodide – Wikipedia,
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