Category: iodides-buliding-blocks

These common heterocyclic compound, 2401-21-0, name is 1,2-Dichloro-3-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. Safety of 1,2-Dichloro-3-iodobenzene

D. 17alpha-Chloro-17beta-Methylsulfinyl-1,4-Androstadiene-3,11-Dione In a manner similar to that described in Example 2A, react 2.4 gm. of 17alpha-methylthio-1,4-androstadiene-3,11-dione, 55.6 ml. of pyridine, 14.4 ml. of water and 5.76 gm. of iodobenzene dichloride. Pass the concentrated residue through a 250 gm. silica gel column, eluding first with chloroform and then with ethyl acetate. Evaporate the ethyl acetate eluates and crystallize from acetone/hexane to obtain the title compound; nmr (CDCl3) delta 1.21 (C13 –CH3, s), 1.45 (C10 –CH3, s), 2.55 (S–CH3, s), 6.10 (C4 –H, d), 6.20 (C2 –H, dd), 7.68 (C1 –H, d).

The synthetic route of 1,2-Dichloro-3-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Schering Corporation; US4183924; (1980); A;,
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Synthetic Route of 111771-08-5, 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. 111771-08-5, name is 2-Fluoro-6-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

Intermediate 14: 2-Fluoro-6-pyrimidin-2-yl-benzoic acid.Step A: 2-Fluoro-6-iodo-benzoic acid methyl ester. To a 200 mL round- bottomed flask were added 2-fluoro-6-iodo-benzoic acid (7.5 g, 28.2 mmol), LiOH?H20 (1 .42 g, 33.8 mmol), and THF (100 mL). The resulting mixture was warmed to 50 C and stirred for 2 h. Dimethyl sulfate (4.03 mL, 42.3 mmol) was then added and the mixture was warmed to 65 C. After 2 h, the mixture was cooled to room temperature and NH4CI(ag) (50 mL, 13 wt% solution) was added. The two resulting layers were thoroughly mixed and then separated. The organic layer was dried over MgS04, filtered, and concentrated under reduced pressure to a light brown oil (7.79 g, 99% yield). 1 H NMR (400 MHz, CDCI3): 7.68 – 7.60 (m, 1 H), 7.15 – 7.06 (m, 2H), 3.98 (s, 3H).

The chemical industry reduces the impact on the environment during synthesis 2-Fluoro-6-iodobenzoic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; LETAVIC, Michael; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHIREMAN, Brock, T.; SWANSON, Devin; WO2012/145581; (2012); A1;,
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Application of 351003-36-6, These common heterocyclic compound, 351003-36-6, name is 2-Fluoro-5-iodobenzonitrile, 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 a stirred solution of terf-butyl frans-4-(4-chlorophenyl)-3- (hydroxymethyl)piperidine-l-carboxylate (2.20 g, 6.75 mmol) in anhydrous N,N- dimethylformamide (100 mL) was added sodium hydride (0.35 g, 8.8 mmol, 60% w/w dispersion in mineral oil) at 0 C. The reaction mixture was stirred at ambient temperature for 30 minutes. 2-Fluoro-5-iodobenzonitrile (1.83 g, 7.40 mmol) was added at 0 C and the reaction mixture was stirred at ambient temperature for 16 h. Saturated ammonium chloride (50 mL) was added, followed by ethyl acetate (200 mL). The organic layer was washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo. The residue was purified by column chromatography (5%-50% gradient of ethyl acetate in hexanes) to afford iert-butyl irans-4-(4-chlorophenyl)-3-((2-cyano-4-iodophenoxy)methyl)piperidine-1-carboxylate in 88% yield (3.30 g) as a colorless solid: MS (ES+) m/z 552.8 (M + 1), 554.8 (M + 1).

The synthetic route of 351003-36-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; XENON PHARMACEUTICALS INC.; SUN, Shaoyi; ZENOVA, Alla, Yurevna; CHAFEEV, Mikhail; JIA, Qi; ZHANG, Zaihui; OBALLA, Renata, Marcella; WO2013/64983; (2013); A1;,
Iodide – Wikipedia,
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6828-35-9, name is 5-Chloro-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. Recommanded Product: 6828-35-9

General procedure: A mixture of 2-iodo aniline/2-iodo phenol (0.25 mmol), Pd-NHC (5 mg, 2 mol%), Mo(CO)6 (0.50 mmol, 132 mg) was taken in round bottomed flask and backfilled with nitrogen three times. Alkyne (0.50 mmol), DMF (2 ml) and Me2NH (4 equiv) were added to the reaction mixture via syringe. The reaction mixture was heated at 95 C until the completion of the reaction. Afterwards, the reaction mixture was poured into the water and extracted with ethyl acetate (3¡Á10 ml). The organic phase was dried over Na2SO4 and concentrated under reduced pressure. The residue was purified through column chromatography using ethyl acetate and petroleum ether as eluents.

The synthetic route of 6828-35-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ghosh, Prasanjit; Nandi, Aritra Kumar; Das, Sajal; Tetrahedron Letters; vol. 59; 21; (2018); p. 2025 – 2029;,
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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. 3058-39-7, name is 4-Iodobenzonitrile, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

General procedure: An oven-dried sealed tube equipped with a magneticstirring bar was charged with aryl iodide (0.65 mmol),Co(OAc)24H2O (15 mol%), l-valine (30 mol%), cesiumcarbonate (2 equiv.), and phenol (0.78 mmol). Acetonitrilesolvent (2.5 cm3) was added and the sealed tube wasevacuated using a vacuum pump, filled with nitrogen,and tightly sealed. It was then stirred in a pre-heated oil bath for 24-48 h. After the completion of the reaction, thereaction mixture was extracted with 15 cm3 of EtOAc andthe EtOAc layer was separated and washed with water.The aqueous layer was collected and further extractedtwo more times with EtOAc (2 ¡Á 15 cm3). The combinedorganic layers were dried over anhydrous Na2SO4andevaporated using a rotatory evaporator. The residue waslater purified by column chromatography (silica 100-200mesh) using hexane-EtOAc mixture as the eluent.

The synthetic route of 3058-39-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ujwaldev, Sankuviruthiyil M.; Saranya, Salim; Harry, Nissy Ann; Anilkumar, Gopinathan; Monatshefte fur Chemie; vol. 150; 2; (2019); p. 339 – 346;,
Iodide – Wikipedia,
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Reference of 460-37-7, 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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under nitrogen protection,Magnesium 13.4g (0.55mol) and magnesium were placed in the reaction flask.3-iodo-1,1,1-trifluoropropane7g is dissolved in 90g of tetrahydrofuran,Slowly raise the temperature to 35-40 C,After the reaction was initiated, 3-iodo-1,1,1-trifluoropropane 105g andA 220 g mixture of tetrahydrofuran was slowly added dropwise to the reaction flask to maintain the temperature at 60-65 C.After the completion of the dropwise addition, the reaction was kept for 2 hours, allowed to stand and cooled to room temperature, and the concentration was measured to be 1.64 mol/L, and the yield was 95%.Under nitrogen protection,2,5 g (0.39 mol) of N,N-dimethylformamide was placed in the reaction flask.2-methyltetrahydrofuran 70g,Cool down to -25 C to -20 C,1.64 mol/L of 1,1,1-trifluoropropyl magnesium iodide was added dropwise in this temperature range.183mL of 2-methyltetrahydrofuran solution, drip, heat for 1 hour, slowly rise to room temperature, add a small amount of water to quench and dissociate, then add 4NHydrochloric acid is adjusted to pH=3-4, and the layer is allowed to stand. The aqueous layer is extracted with a small amount of 2-methyltetrahydrofuran, and the organic phase is enriched and added.And sodium bisulfite was raised to 30-35 C for 1 hour, a large amount of solids were precipitated after cooling, filtered, and the filter cake was rinsed and dried to obtain a solid.The 4,4,4-trifluorobutanal obtained by dissociating the layer and the diluted hydrochloric acid at 35-40 C was dried over anhydrous sodium sulfate to obtain 29.5 g.Yield 78%, GC: 98.6%.

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-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Pulasi Science And Technology (Shanghai) Co., Ltd.; Cai Weibing; Xu Gengdu; (8 pag.)CN109369354; (2019); A;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 116632-39-4, name is 5-Bromo-2-iodotoluene, molecular formula is C7H6BrI, 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. HPLC of Formula: C7H6BrI

Preparation 49 (4-Bromo-2-methyl-phenyl)-(2-methyl-5-nitro-phenyl)-methanone (compound 449) The reaction was run under an argon atmosphere using dry glassware. 4-Bromo-2-methyliodobenzene (2.40 mL, 16.8 mmol) was dissolved in dry THF (15 mL) and cooled to -60 C. Isopropylmagnesium chloride (2 M in THF, 8.4 mL, 16.8 mmol) was added under stirring during 30 minutes. The reaction mixture was allowed to warm up to -40 C. and the mixture was stirred at -40 C. for 4 h. Compound 401 (4.62 g, 16.8 mmol) was added and the mixture was stirred at -40 C. for 3 h after which it was allowed to warm to room temperature and stirred for 17 h. A saturated aqueous solution of NH4Cl (100 mL) was added and the mixture was stirred for 1 h. The phases were separated and the aqueous phase was extracted with EtOAc (2*100 mL). The combined organic phases were washed with brine, dried (MgSO4), filtered and concentrated in vacuo. The crude product was purified by flash chromatography using CH2Cl2/petroleum ether (40-60) 1:6, 1:4, 1:2 as the eluent to afford the title compound as yellow compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 116632-39-4, its application will become more common.

Reference:
Patent; Leo Pharma A/S; US2006/128766; (2006); 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. 74-88-4, name is Iodomethane, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: CH3I

To a solution of 3-iodo-4-hydroxy-5-methoxybenzaldehyde (1.05 g, 3.78 mmol) in CH2Cl2 (50.0 mL) was added aqueous NaOH solution (1.93 g in 30.0 mL of water) and tbutylammonium iodide (2.09 g, 5.66 mmol) and stirred until clear. Methyl iodide (2.80 mL, 45.8 mmol) was added to the reaction mixture and stirred for 12 h at room temperature. The reaction was quenched with 6N HCl, and the organic product was extracted with CH2Cl2, washed with brine, dried, and concentrated to give a solid. The solid was chromatographed (pentane:dichloromethane, 1:1) to give a white solid. (Yield: 957 mg, 3.28 mmol, 87%). 1H NMR (d1-CDCl3, 400 MHz, 20C): delta = 9.81 (s, 1H, C(O)H), 7.83 (d, J = 1.8 Hz, 1H, ArH), 7.39 (d, J = 1.8 Hz, 1H, ArH), 3.91 (m, 6H, 2x OCH3). 13C NMR (d1-CDCl3, 100 MHz, 20C): delta = 189.7, 154.1, 153.0, 134.6, 133.9, 111.1, 92.1, 60.6, 56.1. ESMS calcd for C9H10IO3 [M+H]+ : 292.9669, found 292.9675.

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 74-88-4.

Reference:
Article; Waghorn, Philip A.; Jackson, Mark R.; Gouverneur, Veronique; Vallis, Katherine A.; European Journal of Medicinal Chemistry; vol. 125; (2017); p. 117 – 129;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 51839-15-7, name is Dimethyl 5-iodoisophthalate, molecular formula is C10H9IO4, 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: 51839-15-7

General procedure: A 5 mL microwave glass vial (Biotage) sealable with a septum held in place by a metal crimp cap was charged with a diaryliodonium triflate (0.3 mmol, 1 equiv), an aryl iodide (1.5 mmol, 5 equiv.), and 1,2-dicholoroethane (3 mL, 0.1 M iodonium triflate concentration). The tube was sealed (crimp cap) and submitted to microwave irradiation with a target temperature of 100 C in high absorption mode. After the indicated time, the tube was retrieved and cooled to rt and the contents were concentrated under reduced pressure. The crude material was purified by silica gel flash chromatography (gradient 10 ? 50% acetone/CH2Cl2).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 51839-15-7, its application will become more common.

Reference:
Article; Racicot, Leanne; Ciufolini, Marco A.; Tetrahedron; vol. 73; 50; (2017); p. 7067 – 7072;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 364-75-0, name is 1-Fluoro-4-iodo-2-nitrobenzene, 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 364-75-0, Computed Properties of C6H3FINO2

Example 3-4-3 Preparation of 4-iodo-N-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)-2-nitroaniline To a stirred solution of (3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)methanamine (5.00 g, 18.23 mmol) in acetonitrile (75 mL) was added 1-fluoro-4-iodo-2-nitrobenzene (4.55 g, 17.04 mmol) and diisopropylethylamine (3.30 g, 25.56 mmol). The yellow solution was heated to reflux and stirred. After 4 h, the orange-brown mixture was allowed to cool to room temperature and was diluted with water (150 mL). The resulting bright orange precipitate was isolated by filtration and washed with water. The moist solids were dissolved in dichloromethane, and a small amount of water separated and was removed. The organic phase was dried over magnesium sulfate, filtered, and concentrated to provide 7.10 g (80%) of 4-iodo-N-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzyl)-2-nitroaniline as a bright orange solid.

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-Fluoro-4-iodo-2-nitrobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; KANE, JR., John L.; MATTHEWS, Gloria; METZ, Markus; KOTHE, Michael; LIU, Jinyu; SCHOLTE, Andrew; US2015/158847; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com