Category: iodides-buliding-blocks

Electric Literature of 156150-67-3, The chemical industry reduces the impact on the environment during synthesis 156150-67-3, name is 2-Chloro-1-fluoro-4-iodobenzene, I believe this compound will play a more active role in future production and life.

General procedure: DG1-tetheredalcohol substrate (0.1 mmol), aryl iodide (0.3 mmol), palladium acetate(0.01 mmol), 3-nitro-5-chloro-pyridone (0.04 mmol) and silver trifluoroacetate(0.25 mmol) were added to a 10 ml reaction vial with a magnetic stir bar, themixture was dissolved with 1 ml of HFIP and then the vial was capped. Thereaction mixture was stirred at 100 C for 20 h. The mixture was cooled toroom temperature, diluted with 2 ml of ethyl acetate and filtered through a padof Celite, and then washed with another 2 ml of ethyl acetate. The filtrate wasconcentrated and redissolved with 5 ml of methanol, cooled with an ice bath,and then sulfonyl chloride (0.2 ml) was added slowly. The resulting mixture wasstirred at room temperature for 30 min and then concentrated, the residue waspurified by preparative thin-layer chromatography to get the arylation product.Full experimental details and characterization of compounds are given inthe Supplementary Information.

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, 2-Chloro-1-fluoro-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Xia, Guoqin; Weng, Jiang; Liu, Luoyan; Verma, Pritha; Li, Ziqi; Yu, Jin-Quan; Nature Chemistry; vol. 11; 6; (2019); p. 571 – 577;,
Iodide – Wikipedia,
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Application of 263351-43-5,Some common heterocyclic compound, 263351-43-5, name is tert-Butyl 3-iodobenzylcarbamate, molecular formula is C12H16INO2, 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 solution of the product of preparation 49 (0.75 g, 2.25 mmol), 4-hydroxy phenylboronic acid (0.62 g, 4.50 mmol) and 1, 1′- bis (diphenylphosphino) ferrocenyl palladium (II) chloride (0.11 g, 0.14 mrnol) in N, N-dimethylformamide (14 mL) was treated with 2M aqueous sodium carbonate solution (4 mL) and the resulting mixture was heated at 80 C for 16 hours. The solvent was removed in vacuo and the residue was purified by column chromatography on silica gel, eluting with ethyl acetate: pentane, 25: 75, to afford the title compound as a pale pink crystalline solid in quantitative yield, 0. 73 g. ‘H NMR (400MHz, CDCI3) 8 : 1.47 (9H, s), 4. 33-4. 41 (2H, m), 4. 87-4. 94 (1H, bs), 6.89 (2H, d), 7.21 (1H, d), 7.37 (1H, dd), 7.43-7. 45 (4H, m); LRMS ESI m/z 298 [M-H]-

The synthetic route of 263351-43-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2005/92840; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, molecular formula is C6H3BrINO2, 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: 112671-42-8

Intermediate M1-a (3.7 g, 18.6 mmol)With 2-iodo-5-bromonitrobenzene (15.3 g, 46.7 mmol),Sodium tert-butoxide (7.1g, 74.4mmol), toluene 100mL,Nitrogen protection, Pd2(dba)3(0.3g),Tri-tert-butylphosphine (20ml, 10% toluene solution), stirring turned on,Heated to 100 C reflux, reaction 12h, the reaction solution washed,The organic phase was concentrated and passed through a silica gel column. The eluent was petroleum ether:Ethyl acetate = 50:1, concentrated rinse,Obtain the intermediate M1-b(9.2g, yield 82.7%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 112671-42-8, its application will become more common.

Reference:
Patent; Beijing Dingcai Technology Co., Ltd.; Gu’an Dingcai Technology Co., Ltd.; Fan Hongtao; Xing Qifeng; Zhang Wei; Zhang Xianghui; (28 pag.)CN107880050; (2018); A;,
Iodide – Wikipedia,
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Application of 68507-19-7, A common heterocyclic compound, 68507-19-7, name is 3-Iodo-4-methoxybenzoic acid, molecular formula is C8H7IO3, 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 50 ml_, round-bottom flask equipped with a magnetic stirbar was charged with 3-iodo-4- methoxybenzoic acid (500 mg, 1.97 mmol), HOBT (482 mg, 3.15 mmol) and EDC (567 mg, 2.96 mmol). The reagents were dissolved in 15 ml. CH2CI2 and the solution was allowed to stir for 15 min. Subsequently, isoindoline (0.447 ml_, 3.94 mmol) and TEA (0.819 ml_, 5.91 mmol) were added to the reaction vessel and the solution was allowed to stir for 5 h. Upon completion, the solvent was removed under reduced pressure and the residue was purified via flash chromatography on silica gel to afford 490 mg (65%) of the title compound.

The synthetic route of 68507-19-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; WYETH LLC; LI, David, Zenan; O’NEIL, Steven, Victor; SPRINGER, Dane, Mark; ZEGARELLI, Benjamin, Miller; WO2010/124047; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, Application In Synthesis of 1,5-Diiodopentane

Synthesis of Compound 59.1 [0424] To a solution of tert-butyl 2-(hydroxymethyl)pyrrolidine-l -carboxylate (1.0 g, 4.9 mmol, 1.0 eq) in MeCN (50 mL) were added NaOH (0.39 g, 9.8 mmol, 2.0 eq) and 1, 5- diiodopentane (3.2 g, 9.9 mmol, 2.0 eq). The reaction mixture was stirred at room temperature for 48 h and concentrated under reduced pressure. The residue was diluted with ethyl acetate (100 mL), washed with H20 (100 mL) and brine (50 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column (PE : EA = 5 : 1) to give 59.1 (0.7 g, Y: 36%) as a yellow oil. 1H NMR (400 MHz, CDC13) delta: 3.96-3.92 (m, 1H), 3.54-3.51 (m, 1H), 3.48-3.39 (m, 2H), 3.33-3.32 (m, 3H), 3.19 (t, J = 6.8 Hz, 2H), 2.31-2.19 (m, 1H), 1.95-1.76 (m, 6H), 1.60-1.50 (m, 3H), 1.46 (s, 9H).

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

Reference:
Patent; BIOGEN IDEC MA INC.; JENKINS, Tracy; VESSELS, Jeffery; WO2014/143672; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 127654-70-0, name is 1-Chloro-3-fluoro-2-iodobenzene, 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 127654-70-0, SDS of cas: 127654-70-0

b) 2-chloro-4-fluoro-3-iodo-1-nitrobenzene To a solution of 1-chloro-3-fluoro-2-iodobenzene (15.0 g) in concentrated sulfuric acid (75 mL) was added concentrated nitric acid (5.1 mL) at 0 C., and the mixture was stirred at room temperature for 2 hr. After confirmation of completion of the reaction by TLC, the reaction mixture was poured into ice-cooled water and extracted 3 times with ethyl acetate. The combined organic layer was washed with saturated brine, dried over sodium sulfate and concentrated to give a crude purified product of the title compound (15.0 g). The product was used without further purification for the next step.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Chloro-3-fluoro-2-iodobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Takeda Pharmaceutical Company Limited; FUJIMOTO, Jun; LIU, Xin; KURASAWA, Osamu; TAKAGI, Terufumi; CARY, Douglas Robert; BANNO, Hiroshi; ASANO, Yasutomi; KOJIMA, Takuto; (159 pag.)US2019/169166; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 76801-93-9, The chemical industry reduces the impact on the environment during synthesis 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, I believe this compound will play a more active role in future production and life.

(c) (-)-5-Acetamido-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-isophthalamide The (-)-compound was prepared from (-)-5-amino-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-isophthalamide (14 g) in a similar manner to that described in C(a) above. The product was purified by recrystallisation from water. Yield: 9 g (61%) [alpha]546 =-4.2; [alpha]578 =-3.8 (c=4.5; DMF:H2 O=2:8). Melting point: 287-289 dec. Analysis–Found: C, 25.77; H, 2.72; I, 50.7; N, 5.62. Calc. for C16 H20 I3 N3 O7: C, 25.72; H, 2.70; I, 50.95; N, 5.62.

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, 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nyegaard & Co. A/S; US4250113; (1981); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

61272-76-2, name is 4-Fluoro-2-iodoaniline, 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. COA of Formula: C6H5FIN

7V-Benzyl-5-bromo-2-iodobenzamide (125 mg, 0.30 mmol), 4-fluoro-2-iodoaniline (29 pL, 0.25 mmol), copper(I) iodide (10 mg, 0.05 mmol), and potassium carbonate (86 mg, 0.63 mmol) were taken up in anhydrous DMSO (1.5 mL). The resulting reaction mixture was first stirred at 80 C for 2 hr, followed by heating to 135 C for another 10 hr. After cooling to room temperature, the mixture was diluted with an excess of Et20 and washed with water. The organic layer was dried over NaiSGy filtered and concentrated. The residue was purified by flash column chromatography (EtOAc : Hex = 0 : 100 to 100 : 0; EtOAc : DCM = 0 : 100 to 30 : 70) to give 10-benzyl-2-bromo-8-fluoro-5,10-dihydro-l li7-dibenzo[Z>,e][l,4]diazepin-l l-one (43 mg, 44 %) as a light yellow solid. (0794) NMR (500 MHz, DMSO-de) d 8.06 (s, 1H), 7.74 (d, J = 2.4 Hz, 1H), 7.54 (dd, J = (0795) 2.4, 8.5 Hz, 1H), 7.30 – 7.24 (m, 5H), 7.22 – 7.17 (m, 1H), 7.09 (dd, J= 6.0, 8.7 Hz, 1H), 7.04 (d, ./ 8.9 Hz, 1 H), 6.91 (td, J= 2.7, 8.4 Hz, 1H), 5 26 (s, 2H); LC/MS (ESI) m/z 396.73 [M+H]+.

The synthetic route of 61272-76-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DANA-FARBER CANCER INSTITUTE, INC.; GRAY, Nathanael S.; DE CLERCQ, Dries; JANG, Jaebong; JANNE, Pasi; TO, Ciric; ECK, Michael; PARK, Eunyoung; HEPPNER, David; (0 pag.)WO2019/164949; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, 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 31827-94-8, Computed Properties of C8H6BrIO

General procedure: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

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; Secci, Daniela; Bizzarri, Bruna; Bolasco, Adriana; Carradori, Simone; D’Ascenzio, Melissa; Rivanera, Daniela; Mari, Emanuela; Polletta, Lucia; Zicari, Alessandra; European Journal of Medicinal Chemistry; vol. 53; (2012); p. 246 – 253;,
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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, A new synthetic method of this compound is introduced below., Recommanded Product: 460-37-7

A solution of 2.0 g (5.95 mmol) of the compound from Ex. 21 A in 40 ml DMF was added 1.39 g (13.1 mmol) of cesium carbonate and stirred for 15 min at RT.Then 2.66 g (11.9 mmol) 3,3,3-trifluoro-1-iodopropane were added, and the mixture was heated to 60 C.After 1 hour, additional 2.66 g (11.9 mmol) 3,3,3-trifluoro-1-iodopropane added.Stirring at 60 C was continued for 16 hours.After cooling to RT was treated with about 160 ml of water supply and is extracted three times with 80 ml of diethyl ether.The combined organic extracts were washed with saturated sodium chloride solution.After drying over anhydrous magnesium sulfate, was filtered and evaporated.The crude product was purified by MPLC on a Puriflash cartridge (100 g silica gel, cyclohexane / ethyl acetate 7: 1-> 1: 1).The product fractions were combined, evaporated and the residue dried under high vacuum.There were 1.86 g (72% d. Th.) Of the title compound.

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; BAYER PHARMA AKTIENGESELLSCHAFT; HAERTER, MICHAEL; DELBECK, MARTINA; KALTHOF, BERND; LUSTIG, KLEMENS; LINDNER, NIELS; KAST, RAIMUND; WASNAIRE, PIERRE; SUESSMEIER, FRANK; (372 pag.)TW2016/7950; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com