Iodides-buliding-blocks

Adding some certain compound to certain chemical reactions, such as: 645-00-1, name is 1-Iodo-3-nitrobenzene, 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 645-00-1. 645-00-1

General procedure: Into a reaction glass vial fitted with a magnetic stirring bar anda septum cap penetrated with a syringe needle was added theCo3O4/NGrC-catalyst (2 mol%, 3 wt% Co-phenanthroline oncarbon, 20 mg) followed by the nitro arene (0.5 mmol), theinternal standard (hexadecane, 100 muL), THF (2 mL), and H2O(200 muL). The reaction vial was then placed into a 300 mL autoclave.The autoclave was flushed twice with nitrogen, pressurized with CO at 30 bar pressure. Finally, the autoclave was usedat 60 bar by adding nitrogen and placed into an aluminiumblock, which was preheated at 125 C. After 24 h the autoclavewas placed into a water bath and cooled to r.t. Finally, theremaining gas was discharged, and the samples were removedfrom the autoclave, diluted with EtOAc and analyzed by GC. Todetermine the yield of isolated products, the general procedurewas scaled up by the factor of two, and no internal standard wasadded. After the reaction was completed, the catalyst was filteredoff, and the filtrate was concentrated and purified by silicagel column chromatography (n-heptane-EtOAc mixtures) togive the corresponding anilines.

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 1-Iodo-3-nitrobenzene.

Reference:
Article; Westerhaus, Felix A.; Sorribes, Ivn; Wienhoefer, Gerrit; Junge, Kathrin; Beller, Matthias; Synlett; vol. 26; 3; (2015); p. 313 – 317;,
Iodide – Wikipedia,
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64248-58-4, These common heterocyclic compound, 64248-58-4, name is 1,2-Difluoro-4-iodobenzene, 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.

A. Methyl 1-(3,4-difluorophenyl)-indole-5-carboxylate, 24c. A mixture of methyl indole-5-carboxylate 24a (2 g, 11.4 mmol), 1-iodo-3,4-difluoro-benzene 24b (1.5 mL, 12.5 mmol), CuI (0.22 g, 1.14 mmol), trans-N,N’-dimethylcyclohexane-1,2-diamine (0.54 mL, 3.43 mmol), and K3PO4 (6.06 g, 28.5 mmol) in toluene (12 mL) was heated at 110 C. for 7 hours. The reaction mixture was diluted with CH2Cl2 and filtered. The solution was concentrated and the residue was purified by flash column chromatography (silica gel, 20% EtOAc/heptane) to give 24c (3.0 g).

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 64248-58-4.

Reference:
Patent; Connolly, Peter J.; Macielag, Mark J.; Zhu, Bin; US2012/58986; (2012); A1;,
Iodide – Wikipedia,
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The chemical industry reduces the impact on the environment during synthesis 1878-94-0, name is 2-(4-Iodophenoxy)acetic acid, I believe this compound will play a more active role in future production and life. 1878-94-0

General procedure: Synthetic methods of compounds L1-8 were similar with eachother, we took the synthetic method of the compound L1 for example.A mixture of obtained compound 2 (2 mmol, 0.61 g), phenoxyaceticacid (6 mmol, 0.91 g) and phosphorus oxychloride (15 mL)were added to a 25 mL single-necked flask, then the reaction mixturewas heated to 106 C and refluxed for 7 h. The solvent wasremoved under vacuum distillation and cooled at room temperature.Then the residue was poured into ice-water mixture(400 mL) under stirring. The pH value of the mixture was adjustedto 7-8 with diluted NaOH solution. Then the precipitated solid wasseparated by suction filtration, and washed with water to be neutral.The crude product was dried and added to anhydrous ethanol(100 mL), heated to boiling and separated by suction filtration,purified by washing thoroughly with anhydrous ethanol and driedin vacuum to give the title product L1.

The chemical industry reduces the impact on the environment during synthesis 1878-94-0. I believe this compound will play a more active role in future production and life.

Reference:
Article; Yan, Dong; Xiang, Yu; Li, Kangyun; Chen, Yanwen; Yang, Zehui; Guo, Dongcai; Journal of Molecular Structure; vol. 1074; (2014); p. 487 – 495;,
Iodide – Wikipedia,
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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. 76801-93-9 name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, 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. 76801-93-9

In Example 2, the solution was cooled in a reactor jacket to 70 C immediately after reaching the maximum temperature of approximately 120-125 C. The cooling rate was about 1 C/minute, and the solution was held at 70 C overnight to form over-acetylated Compound A before moving on to the next deacetylation process step to form Compound A. Deacetylation: After acetylation, the reaction solution containing over-acetylated Compound A was concentrated under reduced pressure, before methanol and water was added prior to the deacetylation step. Sodium hydroxide was then added to methanol- water reaction mixture to carry out the deacetylation. The resulting reaction mixture was then further diluted with water before crystallization. Crystallization: To achieve crystallization, hydrochloric acid was first added until the reaction mixture until it was slightly turbid, and then the reaction mixture was seeded with Compound A. The resulting slurry was stirred for 45 minutes before additional hydrochloric acid was added until about pH 7. The slurry was then cooled to 15 C over night. Next day the slurry was filtered, and the filter cake was washed with methanol and then dried in a vacuum oven.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, and friends who are interested can also refer to it.

Reference:
Patent; GE HEALTHCARE AS; SAANUM, Inger, Dagny; HAALAND, Torfinn; KALLEBERG, Rita; WO2015/82719; (2015); A1;,
Iodide – Wikipedia,
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628-21-7, Name is 1,4-Diiodobutane, 628-21-7, 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.

5-Bromo-2- (4-methoxybenzyl) -7-methyliso-1-one at 0 C(3.0 grams, 8.7 moles)N, N-dimethylformamide (30mL)To the solution was added sodium hydride (1.043 g, 43.5 moles).The reaction solution was stirred at room temperature for 10 minutes.Then add 1,5-diiodopentane (3.493 g, 11.3 mol),The reaction solution was stirred at room temperature for 4 hours.After the reaction was monitored by TLC, the reaction was quenched with saturated ammonium chloride solution, and the mixture was extracted with ethyl acetate (100 mL x 2). The organic layers were combined, dried over anhydrous sodium sulfate, filtered and concentrated. The crude product was purified by flash column chromatography (petroleum ether / ethyl acetate = 1/1) to give the product in the form of an oil (1.97 hag, yield 56.8%).

Statistics shows that 1,4-Diiodobutane is playing an increasingly important role. we look forward to future research findings about 628-21-7.

Reference:
Patent; Nuowosida Pharmaceutical Co., Ltd.; Li Bing; (67 pag.)CN110256432; (2019); A;,
Iodide – Wikipedia,
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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. 696-41-3 name is 3-Iodobenzaldehyde, 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. 696-41-3

General procedure: As outlined in Schemes 1 and 2, under anhydrous andanaerobic conditions, ZnCl2 (0.05 mol) was added to themixture of resorcinol (0.1 mol) and chloroacetonitrile (0.12mol) in diethyl ether (50 mL) cooled to 0C. The mixturewas reacted with anhydrous hydrogen chloride gas for 12hours. Intermediate compound 1, chrysin derivatives 2-5were synthesized according to Scheme 2. The Baker-VenKataraman reaction was employed in the synthesis ofchrysin derivatives [31]. 2, 4-dihydroxybenzoyl chloride (86mmol) was obtained after recrystallization with water. 2-Iodobenzaldehyde, 3-iodobenzaldehyde, 2-fluorine-5-iodobenzaldehyde or 3-iodo-4,5-dimethoxy benzaldehyde(12 mmol) and 10% NaOH (20 mL) were added to a solutionof compound 1 (10 mmol) in alcohol (5 mL). The mixturewas stirred at room temperature for 72 hours. Then the solutionwas acidified with 10% aqueous HCl to pH= 7 andstirred for another 48 hours at room temperature. The crudeproduce was purified by column chromatography (ethylacetate/ petroleum ether = 1:1) to get products, compound2: 7-hydroxy-2-(2-iodophenyl)-4H-chromen-4-one yielded62.7%, compound 3: 7-hydroxy-2-(3-iodophenyl)-4Hchromen-4-one yielded 61.5%, compound 4: 2- (2-fluoro-5-iodo- phenyl)-7-hydroxy-4H-chromen-4-one yielded 60.8%,compound 5:7-hydroxy-2-(3- iodo-4,5-di- methoxyphenyl)-4H-chromen-4-one yielded 62.3%. All compounds were yellow products.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Iodobenzaldehyde, and friends who are interested can also refer to it.

Reference:
Article; Wei, Yun; Zheng, Qutong; Tang, Guotao; Song, Chen; Wang, Guan; Zhang, Yinxiang; Xiao, Yan; Zeng, Xianliang; Wang, Zongbao; Xiao, Jichang; Zheng, Xing; Medicinal Chemistry; vol. 12; 5; (2016); p. 441 – 447;,
Iodide – Wikipedia,
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74-88-4, 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. 74-88-4, name is Iodomethane, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of compound2and K2CO3in DMF was added methyl iodide,bromoethaneorbromopentaneand, the resulting mixture was stirred with heating at room temperature for 6h. The mixture was extracted with ethyl acetate, then combined the organicphases,dried(MgSO4) and concentrated under pressure to give the crude product. The crude product was purified by the silica gel column chromatography (petroleum ether /ethyl acetate, 5:1) to give the desired product4a-c.

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:
Article; Wu, Jie; Zhang, Zhi-Hong; Zhang, Lin-Hao; Jin, Xue-Jun; Ma, Juan; Piao, Hu-Ri; Bioorganic and Medicinal Chemistry Letters; vol. 29; 6; (2019); p. 853 – 858;,
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,
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698-70-4, A common heterocyclic compound, 698-70-4, name is 4-Iodo-N,N-dimethylaniline, molecular formula is C8H10IN, 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.

To the solution of 4-iodo-N,N-dimethylaniline2 (1.235 g, 5 mmol) in THF (15 mL), 2-methyl-3-butyn-2-ol (0.6 mL, 6 mmol) and diisopropylamine (2.1 mL, 15 mmol) was added. After stirring the solution under argon at 70 C for 20 min, copper(I) iodide (100 mg, 0.5 mmol) and triphenylphosphine (144 mg, 0.6 mmol) were added. After both reagents have dissolved, palladium(II) acetate (8 mg, 0.035 mmol) was added and stirring was continued for 5 h. Upon cooling, the reaction mixture was filtered and the filtrate was extracted by CH2Cl2. The organic layer was washed with water, dried with sodium sulphate, filtered, and concentrated by rotary evaporation. The crude product was purified by radial chromatography (silica gel, EtOAc/PE = 1/10) to give 4-[4-(dimethylamino)phenyl]-2-methylbut-3-yn-2-ol3 (586 mg, 57%) as yellow crystals: mp 83.0 – 86.5 C. 1H NMR (300 MHz, CDCl3 ) delta (ppm) 1.53 (s, 1H), 1.6 (s, 6H); 2.9 (s, 6H); 6.6 (d, 2H); 7.3 (d, 2H). IR [cm-1] 3329, 2979, 2931, 2222, 1609, 1518.

The synthetic route of 698-70-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rejc, Luka; Fabris, Jan; Adrovi?, Armin; Kasuni?, Marta; Petri?, Andrej; Tetrahedron Letters; vol. 55; 6; (2014); p. 1218 – 1221;,
Iodide – Wikipedia,
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5326-47-6, These common heterocyclic compound, 5326-47-6, name is 2-Amino-5-iodobenzoic acid, 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.

Concentrated H2SO4 (3.7 mL) was added dropwise at 20 C under argon atmosphere to a stirred solution of 5-iodoanthranilic acid (5.0 g, 19 mmol) in MeOH (20 mL), and the mixture was refluxed for 7 h. The mixture was then concentrated in vacuo to the volume of 10 mL, poured into a vigorously stirred saturated solution of NaHCO3 (80 mL), and extracted with EtOAc. The organic layer was washed with a brine solution, dried over Na2SO4, and concentrated in vacuo; the residue was purified by chromatography on SiO2 (eluent was benzene). Ester 6 (3.68 g) was isolated as yellow crystals, m.p. 80-82 C (LP). 1H NMR (CDCl3), delta: 3.87 (s, 3 H, MeO); 5.76 (br.s, 2 H, H2N); 6.46 (d, 1 H, HC(3), J = 8.7 Hz); 7.48 (dd, 1 H, HC(4), J = 8.7 Hz, J = 2.2 Hz); 8.14 (d, 1 H, 2 HC(6), J = 2.2 Hz); which is similar to that reported previously.24

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 5326-47-6.

Reference:
Article; Lozanova; Stepanov; Mel?nik; Zlokazov; Veselovsky; Russian Chemical Bulletin; vol. 68; 1; (2019); p. 64 – 67; Izv. Akad. Nauk, Ser. Khim.; 1; (2019); p. 64 – 67,4;,
Iodide – Wikipedia,
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