Month: July 2021

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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., Formula: C3H4F3I

To a solution of (S)-l-(5-chloro-2-nitrophenyl)-3-methylpiperazine (21 g, 82 mmoL) in DMF (200 niL) was added DIPEA (21 g, 160 mmoL), followed by l ,l,l-trifluoro-3-iodopropane (27.5 g, 123 mmoL). The mixture was stirred at 120 C for 14 h. After cooling to room temperature, the mixture was concentrated at 60 C under high vacuum. The residue was diluted with ethyl acetate (100 mL), washed with water and brine, dried over Na2S04, and concentrated. The residue was purified by silica gel flash column chromatography to give the title compound (15 g, 51.7%). LC/MS m/z = 352.2 [M+l]+.

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 460-37-7.

Reference:
Patent; ARENA PHARMACEUTICALS, INC.; TRAN, Thuy-Anh; KRAMER, Bryan Aubrey; SHIN, Young-Jun; WO2014/182688; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 61272-76-2, These common heterocyclic compound, 61272-76-2, name is 4-Fluoro-2-iodoaniline, 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 flask was charged with Cu2O (14 mg, 0.1 mmol), Cs2CO3 (977 mg, 3 mmol), o-haloaniline (1 mmol) and amidine hydrochloride (1.5 mmol) in 2 mL DMF under nitrogen atmosphere. The mixture was stirred at room temperature and DMEDA (20 mL, 0.2 mmol) was added via syringe. The reaction mixture was then stirred in a preheated oil bath at 140 C for 16 h, and then cooled to room temperature. The inorganic salt was filtered off and ethyl acetate, water was added. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The combined organic layer was dried over Na2SO4, and concentrated in vacuum.The residue was purified by column chromatography on silica gelusing petroleum ether/ethyl acetate as eluent to provide the desired product.

Statistics shows that 4-Fluoro-2-iodoaniline is playing an increasingly important role. we look forward to future research findings about 61272-76-2.

Reference:
Article; Qu, Yanyang; Pan, Lei; Wu, Zhiqing; Zhou, Xiangge; Tetrahedron; vol. 69; 6; (2013); p. 1717 – 1719;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
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. 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 40400-15-5

General procedure: General procedure for indole synthesis by Cu-catalyzed amidation reaction. A dried re-sealable vialwith a Teflon stir bar was charged with amide (3.0 equiv, 1.5 mmol), CuI (5 mol%, 0.025 mmol), K3PO4(2.0 equiv, 1.0 mmol). The vial was sealed with a rubber septum and evacuated and refilled with argonthree times through a syringe needle. Under an argon atmosphere, toluene (0.5 mL),trans-1,2-diaminocyclohexane (20 mol%, 0.1 mmol) and aryl halide (0.50 mmol) were each added viasyringe. The rubber septum was then removed and quickly replaced with a Teflon screw cap and thereaction mixture was stirred at 110 C for 24 h. The resulting suspension was allowed to reach roomtemperature and filtered through a pad of silica gel eluting with AcOEt (10 mL). The filtrate wasconcentrated and the residue was purified by flash chromatography to afford a pure product.

The synthetic route of 40400-15-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Abe, Masahiro; Denneval, Charline; Nozawa-Kumada, Kanako; Kondo, Yoshinori; Heterocycles; vol. 92; 5; (2016); p. 900 – 909;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 351003-36-6,Some common heterocyclic compound, 351003-36-6, name is 2-Fluoro-5-iodobenzonitrile, molecular formula is C7H3FIN, 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.

2-Fluoro-5-iodobenzonitrile (2.0 g, 7.3 mmol) was dissolved in THF (13 mL) and cooled to -35 C., then i-PrMgCl (sol. in THF, 1.5M, 7.3 mL) was slowly added while maintaining the temperature. The mixture was stirred at -25 C. for 1 h and then transferred to a cooled (-70 C.) THF (9 mL) solution of 4-bromobenzoyl chloride (3.20 g, 14.6 mmol). After 1 h stirring at -70 C. the mixture was allowed to slowly attain rt. Concentration and addition of water (100 mL) gave a slurry that was neutralised. Extractive workup (EtOAc, NaHCO3 (aq, sat), brine), drying (Na2SO4) of the combined extracts and concentration furnished, after purification by chromatography, 5-(4-bromobenzoyl)-2-fluorobenzonitrile (1.53 g, 69%).

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

Reference:
Patent; BIS-AROMATIC COMPOUNDS USEFUL IN THE TREATMENT OF INFLAMMATION; US2010/286215; (2010); 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. 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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 188815-32-9, name is 3-Bromo-5-iodobenzoic acid, 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 188815-32-9, Safety of 3-Bromo-5-iodobenzoic acid

To a solution of 3-bromo-5-iodobenzoic acid (53, 500 mg, 1.53 mmol) in methanol (7.5 mL) was added dropwise thionyl chloride (1.1 mL, 2.18 g, 18.35 mmol) at 0 C, and then this reaction mixture was stirred at room temperature for 15 h. After being neutralized with saturated NaHCCb solution on the ice bath, the mixture was extracted with ethyl acetate (20 mL x2). The combined organic layer was washed with brine, dried over MgS04, filtered and evaporated under reduced pressure to afford compound 54 (498 mg, 96%) as a white solid; NMR (400 MHz, CDCb) d 8.32 (t, J =1.40 Hz, 1H), 8.15 (t, J =1.58 Hz, 1H), 8.06 (t, J =1.64 Hz, 1H), 3.95 (s, 3H); MS (ESI, m/z) 340.9, 342.9 [M+l]+; ESI-HRMS calcd. m/z for C8H702I79Br 340.8674, found 340.8672 [M+l]+.

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:
Patent; THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES; JACOBSON, Kenneth A.; YU, Jinha; CIANCETTA, Antonella; WEN, Zhiwei; JUNG, Young-Hwan; (124 pag.)WO2019/157417; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 146137-72-6, 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. 146137-72-6, name is 2-Fluoro-6-iodobenzaldehyde, This compound has unique chemical properties. The synthetic route is as follows.

Step 2: 3-Iodo-1H-pyrazole-4-carbonitrile (3.62 g, 16.5 mmol) was taken up in dry tetrahydrofuran (67 ml) under nitrogen atmosphere. Sodium hydride (992 mg, 24.8 mmol, 60% in oil) was added in one portion and the mixture was placed in a heated (50 C.) sonication bath for 50 minutes. To this mixture was added 2-fluoro-6-iodobenzaldehyde (5.37 g, 21.5 mmol) and the mixture was placed in an oil bath heated to 60-65 C. After 2 hours stirring additional 2-fluoro-6-iodobenzaldehyde (350 mg, 1.4 mmol) was added and the material was stirred for 1 more hour. The flask was cooled to ambient and close to 90% of the solvent was stripped (rotary evaporator). Diethyl ether (30 ml) and water (50 ml) were added and the mixture was vigorously stirred for 30 minutes. The precipitated product was collected by filtration, rinsing well with diethyl ether and water, and drying in a vacuum oven to provide a light tan powder (4.78 g). This solid product was taken up in a solution of 2% methanol in dichloromethane (about 60 ml, heat to dissolve) and transferred to a reparatory funnel. Water (60 ml) was added and the material was shaken and the organic phase collected. This was dried with magnesium sulfate, filtered and stripped to provide the desired 1-(2-formyl-3-iodo-phenyl)-3-iodo-1H-pyrazole-4-carbonitrile as a light yellow powder (3.973 g). LC/MS calc’d for C11H5I2N3O (m/e) 448.99, obs’d 450 (M+H, ES+).

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

Reference:
Patent; Billedeau, Roland Joseph; Kondru, Rama K.; Lopez-Tapia, Francisco Javier; Lou, Yan; Owens, Timothy D.; Qian, Yimin; So, Sung-Sau; Thakkar, Kshitij C.; Wanner, Jutta; US2012/295885; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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 4-Chloro-2-iodobenzoic acid

General procedure: To an oven dried three neck RB containing 2-Iodobenzoic acid (1) (2mmol), benzyl amine (2) (4mmol) and CuI(0.4mmol) in DMSO(3ml) was added 0.55g of K2CO3. Then, the reaction mixture was allowed to stir at 90C under air atmosphere for 12h.The completion of the reaction was monitored by TLC. After being cooled at room temperature the reaction mixture was poured in to ice cooled water and extracted with ethyl acetate two times. The combined organic layer was washed with brine and then dried over anhydrous Na2SO4. The solvent was evaporated and the crude product was purified by column chromatography (hexane(80)/ ethyl acetate (20)) on silica gel to afford 2-phenyl-4H-benzo[d][1,3]oxazine-4-one.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 13421-13-1, its application will become more common.

Reference:
Article; Munusamy, Sathishkumar; Venkatesan, Sathesh; Sathiyanarayanan, Kulathu Iyer; Tetrahedron Letters; vol. 56; 1; (2015); p. 203 – 205;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com