Tag: M.W=400-500

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., Product Details of 63262-06-6

According to the above reaction formula, under nitrogen protection, the purchased 1,4-dibromo-2,5-diiodobenzene (1.00g/2.05mmol),Carbazole (514.29mg, 3.08mmol), potassium hydroxide (230.1mg, 4.10mmol 2,2,6,6-Tetramethyl-3,5-heptanedione (37.80mg, 0.205mmol) and cuprous oxide (29mg, 0.205mmol) were added to 10mL DMF,After heating to 110C for 124 hours, the reaction was extracted three times with 50 ml of saturated brine and 15 ml of dichloromethane.The organic phase was dried over anhydrous sodium sulfate, filtered and concentrated. The crude product was purified by column chromatography using petroleum etherdichloromethane=3:1 (VV) as eluent.1.02 g of white solid product was obtained with a yield of 87.8%.

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; South China University of Technology; Ying Lei; Zhong Zhiming; Li Yuanfeng; Guo Ting; Peng Junbiao; Cao Yong; (11 pag.)CN111116455; (2020); A;,
Iodide – Wikipedia,
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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. Formula: C6H3I3

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;,
Iodide – Wikipedia,
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Application 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.

-78 CCooled titanium-dichloride(Cp 2 TiCl 2, 59.8 mg, 0.24 mmol) in ether (2.4 mL)To the solution was added i-propyl magnesium chloride (2.0 M in ether solution, 0.24 mL, 0.48 mmol)1,4-Dioxane (46 [mu] L, 0.54 mmol)And n-tridecafluorohexyl iodide (C 6 F 13 I, 78 muL, 0.36 mmol) were charged, then the temperature was adjusted to -50 C. and stirred for 2 hours.Subsequently, benzaldehyde (20 muL, 0.20 mmol) was added, the temperature was raised, and the mixture was stirred at room temperature for 1 hour.After completion of the reaction, 1 N hydrochloric acid was added to terminate the reaction, followed by extraction with ether three times. The organic layers were combined, dried over sodium sulfate, filtered, and the solvent was distilled off under reduced pressure to obtain a crude product. The obtained crude product was purified by silica gel column chromatography (hexane / ethyl acetate = 20/1 (v / v)) to obtain 2,2,3,3,4,4,5,5,6, 6,7,7,7-tridecafluoro-1-phenyl-1-hydroxyheptane (85.2 mg, yield:> 99%).

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; TOKYO INSTITUTE OF TECHNOLOGY; TOSOH F-TECH INCORPORATED; MIKAMI, KOICHI; FUJIU, MOTOHIRO; (46 pag.)JP5894739; (2016); B2;,
Iodide – Wikipedia,
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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. 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,4-Dibromo-2,5-diiodobenzene

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

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. 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, A new synthetic method of this compound is introduced below., SDS of cas: 355-43-1

In reaction kettleF (CF2) 6-I(1298.5 kg, 2.911 kmol)Was stirred and stirred.Next, Parroyl IPP[Half-life temperature: 40.3 C]AE-3000 so that 20% by massSolution dissolved in (1,1,2,2-tetrafluoroethyl-2,2,2-trifluoroethyl ether)(17.0 kg, 0.017 kmol)And CH2 = CHCH2 (CH2) 5H (336.5 kg, 2.999 kmol)It was dripped at the said reaction kettle.During dripping,The internal temperature was kept at 88-100 C.After completion of drippingKeep the internal temperature at 90-100 C,As a result of analyzing the reaction crude liquid A1 obtained by further stirring for 0.5 hour or more by gas chromatography,It was confirmed that F (CF2) 6CH2CHICH2 (CH2) 5H was contained.From the obtained reaction crude liquid A1,Under reduced pressure (-0.093 kPaG.Less than,Gauge pressure,?G? is added after ?kPa? or ?MPa?. )AE-3000 and excessCH2 = CHCH2 (CH2) 5HIs distilled off,Reaction solution 1a containing F (CF2) 6CH2CHICH2 (CH2) 5H(1622.4 kg) was obtained.

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; AGC glass company; Maeda, Yutaka; Mitsui, Yoshiyuki; Yamane, Shingo; (11 pag.)JP2019/108319; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 355-43-1, 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.

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.

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, 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, other downstream synthetic routes, hurry up and to see.

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

Electric Literature of 63262-06-6, 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. 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of 2-(tributylstannyl)thiophene (20.7 g, 55.3 mmol) and1,4-dibromo-2,5-diiodobenzene (13.5 g, 27.7 mmol) in dry DMF (100 mL) was addedPd(PPh3)2Cl2 (0.78 g, 1.12 mmol). The mixture was stirred for 40 h at 80 C. Aftercooling to room temperature, the reaction mixture was poured into water and thenextracted with toluene. The combined organic layers were washed with water and driedover anhydrous Na2SO4. After filtration and evaporation, the crude product wasrecrystallized from methanol to provide 8 as a white solid (yield = 10.3 g, 93%).

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, 1,4-Dibromo-2,5-diiodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Komiyama, Hideaki; Adachi, Chihaya; Yasuda, Takuma; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 1459 – 1466;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H2Br2I2

Under nitrogen atmosphere, 1,4-dibromo-2,5-diiodobenzene (3.0 g, 6.2 mmol) was dissolved in diisopropylamine (45 ml) and anhydrous benzene (45 ml), followed by stirring for 30 minutes. Copper iodide (235 mg, 0.12 mmol), PdCl2(PPh3)2 (430 mg, 0.61 mmol), and 1-dodecene (1.9 ml, 12.9 mmol) were added to the mixture, followed by stirring at room temperature for 14 hours. The reaction liquid was poured into water and extracted with chloroform, and the obtained organic layer was washed with 200 ml of water three times. The resulting organic layer was dried over anhydrous sodium sulfate and purified by a column chromatography (silica gel and methylene chloride:hexane = 1:3), followed by recrystallization in ethanol, thereby colorless powdery 1,4-dibromo-2,5-bis(octyne-1-yl)benzene was obtained (1.56 g, yield: 56%). 1H-NMR (400 MHz, CDCL3) delta7.59 (s, 2H) 2.45 (t, J=7.2 Hz, 4H) 1.65-1.23 (m, 32H) 0.88 (t, J=6.4 Hz, 6H)

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; Nippon Kayaku Kabushiki Kaisha; Hiroshima University; EP2147923; (2010); A1;,
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.

Example 3: Synthesis of sodium perfluorohexylsulphinate: C2F5-(CF2-CF2)2-S02Na [5] 52 g (0.3 mol) of sodium dithionite (Na2S204) are added to a jacketed reactor heated using a thermostatically-controlled bath which is equipped with a mechanical stirrer, an upright reflux condenser, a dropping funnel and a temperature probe and which contains 16 g (0.15 mol) of sodium carbonate (Na2C03) dissolved in 480 g of demineralized water. After dissolution, 89.2 g (0.2 mol) ofC6F131, in solution in 120 g of ethanol, are added thereto dropwiseover ‘/2 hour; the two-phase mixture obtained is brought to reflux (76 C) for 1h 30, giving a homogeneous colourless solution. After cooling, this solution is poured onto 180 g of ethyl acetate and 400 g of a saturated aqueous NaCl solution. After separating by settling, the organic phase is washed with a saturated NaCl solution and dried over Na2S04. The solvent is subsequently removed by distillation on a rotary evaporator under reduced pressure. The white solid recovered (79 g, Yd 97%) isC6F13S02Na [5] (MS/negative electrospray: peak at 383 = C6F13SO2-; NMR purity 97%).

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:
Patent; ARKEMA; WO2005/121060; (2005); A1;,
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. 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., Safety of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

2.4. Synthesis of 1-chloro-3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin (Cl-FODMH)3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin (FODMH)was synthesized using similar procedures as in the preparation ofODMH. Briey, 3.20 g DMH were dissolved in 30 mL methanol inthe presence of 1.68 g potassium hydroxide. The mixture was keptat 50 C for 30 min. After evaporation of the solvent, the potassiumsalt of DMH was dried in a vacuum oven at 60 C for three days. Theanhydrous salt was then dispersed in 100 mL N,N-dime-thylformamide (DMF) at 95 C for 10 min under constant stirring,after which 11.85 g IFO were added into the mixtures. The reactionwas continued for 4 h at 95 C. At the end of the reaction, theformed KI was ltered off. After the removal of DMF by distillationunder reduced pressure, the residual substance was recrystallizedfrom ethanol. 3-1H,1H,2H,2H-perurooctyl-5,5-dimetylhydantoin(FODMH) was obtained as white powders with a yield of 60.7%(7.22 g).In the preparation of Cl-FODMH, 0.5 g FODMH and 0.74 g tri-chloroisocyanuric acid (TCCA) were dissolved in acetone [10]. Here,TCCA was employed because our screening tests showed that usingchlorine bleach as the chlorination agent could not chlorinateFODMH successfully due to the very hydrophobic nature ofFODMH. The solution was vigorously stirred for 30 min at ambienttemperature. At the end of the reaction, acetone was evaporated,hexane was added to the mixtures, and the insoluble solids wereltered off. After removing hexane from the ltrate by evaporation,Cl-FODMH was obtained as white powders with a yield of 59.2%.

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

Reference:
Article; Lin, Jiajin; Jiang, Fuguang; Wen, Jianchuan; Lv, Wei; Porteous, Nuala; Deng, Ying; Sun, Yuyu; Polymer; vol. 68; (2015); p. 92 – 100;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com