Tag: M.W=300-400

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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 328-73-4

General procedure: Diarylzinc reagents were generated in situ as described below. In all reactions, 1 equiv of diarylzinc reagent was used except for reactions with diphenylzinc reagent, where only 0.5 equiv was used.In a glovebox, ZnCl2 (136.3 mg, 1.0 mmol) and aryllithium (2.0 mmol) were weighed into a 4-dram and a 1-dram vial, respectively. Then a solution of aryllithium in THF (2 mL) was added dropwise to the suspension of ZnCl2 in THF (2 mL) at r.t. The mixture was stirred for 1 h, THF was removed, and the in situ generated diarylzinc reagent was dissolved in DMF (5 mL). CuI (9.5 mg, 0.050 mmol), aryl halide (1.0mmol), and LiCl (42.3 mg, 1.0 mmol) were weighed into a 15-mL pressure vessel and the diarylzinc reagent was added. The pressure vessel was then tightly capped, taken out of the glovebox, and placed in an oil bath preheated to 100 °C with vigorous stirring. After 12 h, the mixture was cooled to r.t., diluted with EtOAc (15 mL) and washed with H2O (3 × 5 mL); the aqueous fraction was back-extracted with EtOAc (3 × 5 mL). All of the EtOAc extracts were combined and dried (Na2SO4), and the solvent was removed on a rotary evaporator. The product was purified by column chromatography (silica gel, 0?10 percent EtOAc?hexanes).

According to the analysis of related databases, 328-73-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Thapa, Surendra; Vangala, Adarsh S.; Giri, Ramesh; Synthesis; vol. 48; 4; (2016); p. 504 – 511;,
Iodide – Wikipedia,
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Reference of 51560-21-5, 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. 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a 10 mL headspace crimp vial equipped with a magnetic stirrer the corresponding styrene (2.0 mmol), aryl 1,4-dihalide precursor (1.0 mmol), bis(dibenzilidene)acetone palladium (0) (2.0 mol%) and triphenylphosphite (9.0 mol%) were added. The vial was then sealed with a PTFE septum and an aluminum cap followed by purge-saturation with argon. Dry DMF (3 mL) and triethylamine (2.0 mmol) were subsequently added via syringe. The reaction mixture was stirred at 110C for 24 hours. After reaction is complete, the crude was filtered over celite and precipitation of the product was induced by addition of cold water (75 mL). Recrystallization from a 2:1 DMF:1,4-dioxane afforded the desired OPVs.

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-Diiodo-2,5-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Acelas, Mauricio; Sierra, Andres Felipe; Sierra, Cesar A.; Synthetic Communications; (2020);,
Iodide – Wikipedia,
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Electric Literature of 112671-42-8, The chemical industry reduces the impact on the environment during synthesis 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, I believe this compound will play a more active role in future production and life.

A sealed tube was charged with CuI (0.19g, 1.0mmol, 2.5 equiv.), AgF (0.13g, 1.0mmol, 2.5 equiv.), pyridine (0.27mL, 8.3 equiv.), various iodoarenes (0.4mmol, 1.0 equiv.), triethyl(1,1,2,2-tetrafluorobut-3-en-1-yl)silane (4 : 0.19g, 0.8mmol, 2.0 equiv.) and DMF (3.2mL, 0.25M) in glove box. The sealed tube was brought under an atmosphere of argon and capped. The resulting mixture was stirred at 60C for 16h, and then cooled room temperature. The resulting mixture was passed through short column. The eluent was concentrated in vacuo to give the crude materials, which were purified by silica gel column chromatography, leading to the desired coupling products

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, 4-Bromo-1-iodo-2-nitrobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Yakushijin, Ryosuke; Yamada, Shigeyuki; Konno, Tsutomu; Journal of Fluorine Chemistry; vol. 225; (2019); p. 35 – 43;,
Iodide – Wikipedia,
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Synthetic Route 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.

A solution of 3,4-difluoro-2-[(2-fluoro-4-iodophenyl)amino]benzoic acid (201 mg, 0.512 mmol), prepared using procedures similar to those described in US 7,019,033, 3- (2-aminopyrimidin-4-yl)azetidin-3-ol (87 mg, 0.52 mmol), benzotriazol-1-yl-oxy- tris(pyrrolidino)phosphonium hexafluorophosphate (293 mg, 0.563 mmol) and lambdazetaiV-diisopropylethylamine (270 uL, 2.82 mmol) in lambdazetaN-dimethylformamide (2 mL) was stirred at room temperature for 2Oh. The mixture was partitioned between ethyl acetate and saturated sodium bicarbonate. The organic layer was separated and washed with brine, dried over sodium sulfate, filtered and the filtrate concentrated in vacuo. The residue was purified by reverse phase HPLC to afford the title compound 3-(2-aminopyrimidin-4-yl)-l-({3,4- difluoro-2-[(2-fluoro-4-iodophenyl)amino]phenyl}carbonyl)azetidin-3-ol (22 mg, 7%). 1H NMR (400 MHz, CD3OD): 8.23-8.20 (d, IH), 7.48-7.43 (d, IH), 7.35-7.32 (m, 2H), 7.09- 7.00 (m, IH), 6.88-6.84 (d, IH), 6.70-6.63 (t, IH), 4.59-4.54 (d, IH), 4.45-4.40 (d, IH), 4.23- 4.18 (d, IH), 3.04-3.99 (t, IH); MS (EI) for C20Hi5F3IN5O2: 542 (MH+).

The synthetic route of 391211-97-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EXELIXIS, INC.; WO2007/44515; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 181765-86-6,Some common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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.

500mL round-bottom flask reactor, methyl 5-bromo-2-iodo benzoate (25.0g, 73mmol) in 4-dibenzofuran boronic acid (18.7g, 88mmol), tetrakis (triphenylphosphine) palladium (1.7g, 0.15mmol), potassium carbonate (20.2 g, 146.7mmol) put the toluene 125 mL, tetrahydrofuran 125mL, water 50 mL. The temperature of the reactor was 80 C, 10 hours was stirred. When the reaction is complete cool down the temperature of the reactor to room temperature, extracted with ethyl acetate and the organic layer was separated It was. The organic layer was concentrated under reduced pressure and separated by column chromatography to give the intermediate 1-a. (75.0g, 60.1%)

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

Reference:
Patent; SFC CO LTD; PARK, SEOK BAE; SONG, JU MAN; LEE, YUR IM; KIM, HEE DAE; PARK, SANG WOO; JEONG, KYUNG SEOK; CHA, SOON WOOK; (96 pag.)KR2015/130206; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 791642-68-7,Some common heterocyclic compound, 791642-68-7, name is 4-Bromo-1-iodo-2-methoxybenzene, molecular formula is C7H6BrIO, 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.

(Reference Example 4) 1-(4′-bromo-2′-methoxy-[1,1′-biphenyl]-4-yl)cyclopropanecarboxylic acid ethyl ester A 1,4-dioxane (15 ml)-water (10 ml) solution of 1.2 g (3.8 mmol) of 4-bromo-1-iodo-2-methoxybenzene synthesized in analogy to Reference Example 3, 1.1 g (3.5 mmol) of 1-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]cyclopropanecarboxylic acid ethyl ester (synthesized in accordance with the process described in ) and 1.1 g (10 mmol) of sodium carbonate was degassed and was purged with nitrogen. Next, 0.10 g (0.12 mmol) of [1,1′-bis(diphenylphosphino)ferrocene]palladium (II) dichloride methylene chloride adduct was added. The mixture was stirred in a nitrogen atmosphere for 1.5 hours while performing heating at 80C. After the completion of the reaction, water was added to the reaction mixture liquid, and the mixture was extracted with ethyl acetate. The organic phase was washed with saturated brine, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (eluting solvent: hexane:ethyl acetate = 94:6 to 75:25 (V/V)), and the fraction containing the target compound was concentrated under reduced pressure and was dried by vacuum heating to give the title compound weighing 0.72 g (1.9 mmol, yield 55%) as a white solid. Mass spectrum (EI, m/z): 374 [M]+. 1H-NMR spectrum (400MHz, CDCl3) delta: 7.45-7.41 (2H, m), 7.39-7.35 (2H, m), 7.19 (1H, d, J = 8.0 Hz), 7.15 (1H, dd, J = 8.0, 1.8 Hz), 7.10 (1H, d, J = 1.8 Hz), 4.12 (2H, q, J = 7.1 Hz), 3.81 (3H, s), 1.61 (2H, dd, J = 7.0, 4.0 Hz), 1.22 (2H, dd, J = 7.0, 4.0 Hz), 1.19 (3H, t, J = 7.1 Hz).

The synthetic route of 791642-68-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UBE Industries, Ltd.; IWASE, Noriaki; NISHIDA, Hiroshi; OKUDO, Makoto; ITO, Masaaki; KONO, Shigeyuki; MATOYAMA, Masaaki; USHIYAMA, Shigeru; OKANARI, Eiji; MATSUNAGA, Hirofumi; NISHIKAWA, Kenji; KIMURA, Tomio; (54 pag.)EP3162801; (2017); 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. 260355-20-2, name is 1-Chloro-4-iodo-2-(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H3ClF3I

Ethyl 1 H-pyrazole-4-carboxylate (20 g), 1-chloro-4-iodo-2 – (trifluoromethyl) benzene (44 g)Copper iodide (2.7 g),(1 S, 2 S) -N 1, N 2 -dimethylcyclohexane-1, 2-diamine (3.0 g)Sodium ascorbate (2.8 g), sodium carbonate (30 g)In dimethylsulfoxide (80 mL) was stirred at 150 C. for 6 hours.After cooling at room temperature, the reaction solution was added to toluene (0.45 liter), And 10% saline (0.50 l) was added thereto, followed by stirring at room temperature for 30 minutes.After insoluble matter was filtered off with Celite (registered trademark), the two layers were separated.The aqueous layer was extracted with toluene (0.20 l), and the combined organic layer was washed with 10% brine (0.30 l) and then dried over anhydrous magnesium sulfate.The solvent was distilled off under reduced pressure, and the obtained residue was purified by OH type silica gel column chromatography (hexane: ethyl acetate = 90: 10 ? 25: 75) to give the title compound (23 g) as a pale red solid It was

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 260355-20-2.

Reference:
Patent; TAISHO PHARMACEUTICAL COMPANY LIMITED; KAWABE, KENICHI; YAMAMOTO, KUMIKO; UNEUCHI, FUMITO; ASANUMA, YUTA; YAMAGUCHI, CHITOSE; USHIKI, YASUNOBU; SHIBATA, TSUYOSHI; OHTA, HIROSHI; (254 pag.)JP2018/83767; (2018); A;,
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. 199850-56-1, name is Methyl 2-amino-4-chloro-5-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 199850-56-1

Intermediate 41 : Methyl 4-amino-4′-bromo-6-chloro-3-biphenylcarboxylateA suspension of methyl 2-amino-4-chloro-5-iodobenzoate (Intermediate 2) (8.2 g, 26.3 mmol), (4-bromophenyl)boronic acid (5.29 g, 26.3 mmol), tetrakis(triphenylphosphine) palladium (0.304 g, 0.263 mmol) and sodium carbonate (79 ml_, 1 M in water, 79 mmol) in 1 ,4-dioxane (300 ml_) was stirred 3 days at 80C. After cooling, the mixture was filtered through celite, the filtrate was then diluted with water and extracted twice with dichloromethane. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was triturated in diisopropylether, filtered and washed with acetonitrile then diisopropylether to give the title compound methyl 4-amino-4′-bromo-6- chloro-3-biphenylcarboxylate (2.5 g, 7.34 mmol, 27.9% yield) as an off-white powder. LCMS: (M+H)+ = 340-342 ; Rt = 4.09 min.

The synthetic route of 199850-56-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE LLC; DAUGAN, Alain Claude-Marie; LAMOTTE, Yann; MIRGUET, Olivier; WO2012/119978; (2012); A1;,
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. 62720-29-0, name is 1,3-Dibromo-5-fluoro-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C6H2Br2FI

Example 104k 2,6-Dibromo-4-fluorobenzaldehyde 104k To a solution of 1,3-dibromo-5-fluoro-2-iodobenzene (50 g, 132 mmol) in anhydrous toluene (300 mL) cooled at -35 C. was added a solution of isopropyl-magnesium chloride (84 mL, 171 mmol, 2.0M in Et2O) over 30 minutes while maintaining the internal temperature below -25 C. A clear brown solution was obtained and the stirring was continued for 1.5 h at -25 C. Then anhydrous DMF (34 mL, 436 mmol) was added over a period of 30 minutes. The reaction mixture was warmed to 10 C. (room temperature) over 1 h and stirred at this temperature for 1.5 h (hours). It was then quenched with 3.0M HCl and followed by the addition of ethyl acetate. The organic layer was separated and evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with petroleum ether/ethyl acetate (from 50:1 to 20:1) to give 104k as a white solid (20 g, 54%). 1H NMR (500 MHz, CDCl3) delta 10.23 (s, 1H), 7.48 (d, J=7.5, 2H).

The synthetic route of 62720-29-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GENENTECH, INC.; Crawford, James John; Young, Wendy B.; US2013/116245; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 98-61-3,Some common heterocyclic compound, 98-61-3, name is 4-Iodobenzenesulfonyl chloride, molecular formula is C6H4ClIO2S, 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.

p-Iodobenzenesulfonyl chloride (9.08g, 0.03mol), 10mL acetonitrile and 30mL water were added into a 100-mL round-bottomed flask. Then around 15mL of NH3 gas was bubbled into the mixture. The solution was refluxed for 8h at 100C, and the volatile material was removed using a rotary evaporator. The solid crude product was then re-crystallized from a water solution and filtered. The pure product 7.64g of p-iodobenzenesulfonyl amide 1 was obtained with a yield of 90% after drying under high vacuum for 2h. (0015) Alternatively, in a 250-mL three-necked round bottom flask, p-iodobenzenesulfonyl chloride (9.08g, 0.03mol) was added. Then ca. 30mL of ammonia was condensed into the flask at -60C and the flask was allowed to slowly warm to room temperature over 8h. The crude product was washed with 40mL water and dried under the vacuum to give 8.07g purified amide 1 with a yield of 95%. 1H NMR (CD3CN, ppm): (ab, deltaa 7.89 (2H, d), deltab 7.60 (2H, d), Jab=10Hz, deltac 5.70 (2H, s) (0018) (note: The 1H for this and related compounds represents an aa?bb? spin system but it appears as a deceptively simple ab system with J/delta near 0.5. The deltaa,b for all compounds are taken as the midpoint of the second order doublets as an approximation as if it is a classic ab spin system. The Ja,b is assigned as that of a classic ab spin system. No effort was made to analyze the spectra further.)

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

Reference:
Article; Mei, Hua; Desmarteau, Darryl D.; Journal of Fluorine Chemistry; vol. 160; (2014); p. 12 – 15;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com