Category: iodides-buliding-blocks

Related Products of 391211-97-5,Some common heterocyclic compound, 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, molecular formula is C13H7F3INO2, 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.

EXAMPLE 1 1-3. 4-DIFLUORO-2- (2-FLUORO-4-IODO-PHENVLAMINO)-PHENVLL-2-HYDROXV-ETHANONE To a stirring suspension comprised of 3, 4-DIFLUORO-2- (2-FLUORO-4-IODO-PHENYLAMINO)- benzoic acid (1.33 g, 3.4 MMOL, which can be prepared according to the procedure of WO 02/06213) and oxalyl chloride (1.4 mL, 16 mmoles) in dichloromethane (10 mL) at ambient temperature was added 0.025 mL OF N, N-DIMETHYLFORMAMIDE. The reaction mixture was stirred for ten minutes and was concentrated in vacuo to the yellow solid 3, 4-DIFLUORO-2- (2- FLUORO-4-IODO-PHENYLAMINO)-BENZOYL chloride. The yellow solid was suspended in tris (trimethylsiloxy) ethylene (10 g, 33 MMOL) and the stirring mixture was brought to 90 C under a nitrogen atmosphere for six hours. The mixture was cooled slightly, and to it was added a solution consisting of dioxane (25 mL) and 10% aqueous hydrochloric acid (10 mL). Vigorous liberation of gas ensued and the mixture was stirred for ten minutes at 85 C. Brine (50 mL) was added and the mixture was extracted twice with ether (2 x 150 mL). The combined ether phases were washed twice with saturated aqueous sodium bicarbonate (2 x 150 mL). The ether phase was dried (MGS04) and was concentrated in vacuo to 1.4 g of an orange oil that was purified by flash chromatography. Elution with a gradient (100% hexanes to 1: 3 hexanes/ethyl acetate over 72 minutes) afforded a solid with minor impurities. The solid was dissolved in dichloromethane and vacuum filtered through silica to afford 0.135 g (9.8 % yield over two steps) of a yellow solid ; mp 128-128.5 C ; H-NMR (400 MHz; CDCl3) IB 9.80 (s, 1H), 7.40 (m, 3H), 6.77 (m, 2H), 4.83 (d, 2H, J=3.9 Hz), 3.44 (t, 1 H, J=4.1 Hz) ; 19F- NMR (376 MHz; CDCl3) 6-124. 52 (t, 1F, J=10.1 Hz), -125.27 (dd, 1F, J=10.1, 5.1 Hz), – 144.11 (d, 1F, J=7.7 Hz); MS (APCI+) 407.8 (M+1, 28), 389.8 (100); (APCI-) 405.8 (M-1, 100), 402.8 (53); IR 1662,1529, 1503,1260, 1067 CM~1 ; % C (calculated for C14H9F31NO2/FOUND) 41.30/41. 52, % H 2.23/2. 08, % N 3.44/3. 45.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, its application will become more common.

Reference:
Patent; WARNER-LAMBERT COMPANY LLC; WO2005/7616; (2005); A1;,
Iodide – Wikipedia,
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Reference of 1829-28-3,Some common heterocyclic compound, 1829-28-3, name is Ethyl 2-iodobenzoate, molecular formula is C9H9IO2, 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.

In a two-necked round-bottomed flask, equipped with a teflon-coated stirrer bar and reflux condenser, was added ethyl 2-iodobenzoate (3j, 0.14 g 0.50 mmol), Cu2O (0.060 g, 0.42 mmol), and a DMF solution of 2-Zn (0.65 M, 1.54 mL, 1.0 mmol), and the mixture was stirred at 100 C for 24 h. After being cooled to room temperature, the resulting solution was subjected to a short pad of silica gel using hexanes as an eluent. The filtrate was concentrated in vacuo to give the crude materials, which was purified by silica gel column chromatography to provide the corresponding compound 4j (0.13 g, 0.48 mmol) in 96percent yield as an yellow oil. Ethyl 2-(1,1,2,2-tetrafluorobut-3-en-1-yl)benzoate (4j) Yield: 96percent (0.13 g, 0.48 mmol); Yellow oil (hexanes/AcOEt = 15/1, Rf = 0.29); 1H NMR (CDCl3): 1.35 (t, J = 7.1 Hz, 3H, CH2CH3), 4.36 (q, J = 7.1 Hz, 2H, CH2CH3), 5.70 (d, J = 11.0 Hz, 1H, trans-CH2CHCF2), 5.86 (dt, J = 17.3, 2.2 Hz, 1H, cis-CH2CHCF2), 6.07 (ddt, J = 17.3, 11.4, 11.0 Hz, 1H, CF2CH), 7.47?7.62 (m, 4H, ArH); 13C NMR (CDCl3): 14.1 (CH2CH3), 61.9 (CH2CH3), 115.2 (tt, J = 250.2, 37.2 Hz, CF2), 116.6 (tt, J = 253.4, 36.1 Hz, CF2), 124.2 (t, J = 9.3 Hz, CH2), 126.8 (t, J = 24.4 Hz, CF2CH), 127.7 (t, J = 24.5 Hz, Ar), 128.5 (Ar), 128.7?128.9 (m, Ar), 129.7(Ar), 131.1 (Ar), 133.8 (t, J = 3.3 Hz, Ar), 168.6 (C=O); 19F NMR (CDCl3): 106.44 (s, 2F, CF2Ar), 113.42 (d, J = 11.4 Hz, 2F, CF2CH); IR (neat): 3076, 2988, 2903, 1739, 1578, 1415, 1370, 1269, 1152 cm-1 ; HRMS (FAB) calcd for [M+H]+ C13H13F4O2: 277.0852, found 277.0847.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 2-iodobenzoate, its application will become more common.

Reference:
Article; Tamamoto, Ken; Yamada, Shigeyuki; Konno, Tsutomu; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 2375 – 2383;,
Iodide – Wikipedia,
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Reference of 21740-00-1,Some common heterocyclic compound, 21740-00-1, name is 5-Bromo-2-iodobenzoic acid, molecular formula is C7H4BrIO2, 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 a stirred mixture of acid 2-iodo-5-bromobenzoic acid (15.0 g, 45.9 mmol) in dry THF (100 mL) under argon was added neat BH3.DMS (16.0 mL, 169 mmol) dropwise over 20 minutes. The resulting mixture was heated at 65 C. for 8 hours, cooled to room temperature and quenched by the dropwise addition of water (40 mL). The reaction mixture was concentrated in vacuo. The crude alcohol was diluted with of EtOAc (300 mL), washed with 1N NaOH (2¡Á30 mL), 1N HCl (1¡Á30 mL), saturated aqueous NaHCO3 solution (1¡Á30 mL) and brine (1¡Á30 mL). The EtOAc layer was dried (MgSO4), filtered and concentrated in vacuo to give 2-iodo-5-bromobenzyl alcohol (13.8 g, 96%). 1H NMR (CDCl3): delta 7.56 (d, 1H, J=8.25 Hz), 7.54 (s, 1H), 7.04 (d, 1H, J=8.25 Hz), 4.47 (s, 2H). HPLC: Rt=3.12 min. m/z=312 M+H+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Bromo-2-iodobenzoic acid, its application will become more common.

Reference:
Patent; Fink, Brian E.; Gavai, Ashvinikumar V.; Vite, Gregory D.; Han, Wen-Ching; Misra, Raj N.; Xiao, Hai-Yun; Norris, Derek J.; Tokarski, John S.; US2005/250753; (2005); A1;,
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. 626-01-7, name is 3-Iodoaniline, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C6H6IN

General procedure: In a 10-ml round-bottom flask equipped with a condenser, a mixture of the aromatic amine (2 mmol), ethyl acetoacetate (1 mmol), and [Pyridinium-SO3H]HSO4 (0.0,385 g, 15 mol %) was stirred at 100 C for 10 min. Afterwards, the aromatic aldehyde (2 mmol) was added, and the resulting mixture was kept under stirring for the specified time in Table 3, the progress of the reaction was followed by TLC. After completion of the reaction, the reaction mixture was cooled to room temperature, extracted by the warm EtOAc (10 ml) to separate the catalyst. EtOAc was removed and the crude product was recrystallized from aqueous ethanol (96 %) to afford the pure product, which required no further purification. The recovered catalyst was washed with EtOAc (2 x 10 ml), dried, and reused, without considerable catalytic activity decrease.

According to the analysis of related databases, 626-01-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Mohammadi, Sedigheh; Abbasi, Mohsen; Research on Chemical Intermediates; vol. 41; 11; (2015); p. 8877 – 8890;,
Iodide – Wikipedia,
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Application of 32024-15-0, 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. 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

13as) In analogy to Example 13ap), from 3-iodo-4,5-dimethoxy-benzaldehyde and hydroxylamine hydrochloride there is obtained the corresponding 3-iodo-4,5-dimethoxy-benzaldehyde oxime as a colourless solid. Yield: 99%.

The synthetic route of 3-Iodo-4,5-dimethoxybenzaldehyde has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; US5763450; (1998); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 450412-28-9, name is 1-Bromo-3-chloro-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 450412-28-9, Recommanded Product: 1-Bromo-3-chloro-2-iodobenzene

Step 1: 1-bromo-3-chloro-2-cyclopropylbenzene The mixture of 1-bromo-3-chloro-2-iodobenzene (7 g, 22.1 mmol), cyclopropylboronic acid (3.8 g, 44.2 mmol), Pd (dppf) Cl 2 (1.6 g, 2.21 mmol) and K 2CO 3 (2 g, 7.3 mmol, 1.0 eq) in dioxane (100 mL) was heated at 70 C for 12 hours under N 2 protection. TLC showed the reaction was complete and a new spot formed. The mixture was cooled to room temperature and was diluted with EtOAc (150 mL) and H 2O (50 mL). The organic phase was separated and washed with water (150 mL), brine (150 mL), dried over Na 2SO 4, and concentrated. The residue was purified by column chromatography on silica gel (eluent: PE) to give 1-bromo-3-chloro-2-cyclopropylbenzene (3 g, crude), which was used directly in next step.

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Reference:
Patent; BEIGENE, LTD.; GUO, Yunhang; XUE, Hai; WANG, Zhiwei; SUN, Hanzi; (493 pag.)WO2019/210828; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 3032-81-3, A common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, molecular formula is C6H3Cl2I, 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 suspension of DL-5-methoxypyrrolidin-2-one (3a) or arylaminopyrrolidinones 3b,c (1 equiv), CuI (0.5 equiv), cesium carbonate (2 equiv), and corresponding aryl iodide (1 equiv) in dioxane was placed under a nitrogen atmosphere. The coupling ligand DMEDA (1 equiv) was added dropwise by using a syringe and the mixture was then stirred at 60 ¡ãC for various periods of time (14?88 h). At the end ofthe reaction, the insoluble salts deposited after cooling at r.t. were collected by filtration then washed with dichloromethane. The resulting filtrate was concentrated in vacuo and the residue was partitioned between water and dichloromethane. The organic layer was dried on MgSO4 and evaporated to dryness. The residue was finally purified by chromatography on silica gel column (EtOAc/n-heptane) to afford pure N-arylated compound 40?44.

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Baudelet, Davy; Daich, Adam; Rigo, Benoit; Lipka, Emmanuelle; Gautret, Philippe; Homerin, Germain; Claverie, Christelle; Rousseau, Jolanta; Abuhaie, Cristina-Maria; Ghinet, Alina; Synthesis; vol. 48; 14; (2016); p. 2226 – 2244;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C6H5ClIN

A solution of 3-CHLORO-4-IODO-ANILINE (5. 6G), ISOAMYLNITRITE (8. 8ML) and ETHYLDISULPHIDE (13. 4ML) in acetonitrile (100ml) was heated at 60C for 24h. The solvent was removed under reduced pressure and the residue purified by chromatography on silica eluting with 1% ETHYLACETATE/ISOHEXANE. YIELD 4. 02G ‘H NMR CDC13 : 8 7. 70 (1H, D) ; 7. 36 (1H, d); 6. 87 (1H, dd); 2. 94 (2H, q) ; 1. 32 (3H, t)

The synthetic route of 135050-44-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2004/89885; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 83863-33-6, These common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-methylaniline, 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.

9.97 g of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide (30.3 mmol) and 5.03 g of potassium iodide (30.3 mmol) in 75 ml. of cyclohexanol were stirred for 1 h at 800C. After addition of 7.7 g of sodium carbonate (72.7 mmol) and 5.65 g of 5-iodo-2-methyl- aniline (24.2 mmol), stirring continued for deltah at 1600C. At room temperature, the mixture was filtered, washed with dichloromethane, and the filtrate evaporated to dryness. The residue was dissolved in dichloromethane, filtered, and the solvent evaporated. The remaining residue was trituated with n-heptane and the crystalline product filtered off, washed several times with n-heptane and dried in vacuo to yield 10.7 g of product

The synthetic route of 83863-33-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBOTT GMBH &; CO. KG; ABBOTT LABORATORIES; HAUPT, Andreas; POHLKI, Frauke; DRESCHER, Karla; WICKE, Karsten; UNGER, Liliane; RELO, Ana-Lucia; BESPALOV, Anton; VOGG, Barbara; BACKFISCH, Gisela; DELZER, Juergen; ZHANG, Min; LAO, Yanbin; WO2010/125134; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 61272-76-2 as follows. name: 4-Fluoro-2-iodoaniline

General procedure: A 25 mL Wattecs reaction tube was charged with 2-haloaniline 1 (0.6 mmol), potassium O-ethyl dithiocarbonate 2 (1.8 mmol),CuCl (0.06 mmol), and DMF (2 mL). The reaction vessel was flushed with argon three times and sealed. Then the mixture was stirred electromagnetically in an oil bath at 110¡ãC for 6 h.The reaction process was monitored by TLC on silica gel. After the reaction was completed, the reaction mixture was cooled to room temperature, and then HCl (3 mL, 3 mol/L) was added and stirred for another 30 min. The reaction mixture solution was extracted by ethyl acetate (3 ¡Á 20 mL). Subsequently, the combined organic solutions were dried by anhydrous sodium sulfate and the target product was purified by chromatography on a silica gel column (eluent: petroleum ether/ethyl acetate) togive the corresponding pure product 3. Complete characterization characterizationof the products (all known) is found in the Supplemental Materials (Figures S1?S13).

According to the analysis of related databases, 61272-76-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Lei; Zhu, Ning; Gao, Min; Zhao, Xiaole; Han, Limin; Hong, Hailong; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 191; 5; (2016); p. 699 – 701;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com