Category: iodides-buliding-blocks

181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, 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. HPLC of Formula: C8H6BrIO2

Methyl 500mL round bottom flask reactor, 5-bromo-2-iodo benzoate (20.0g, 59mmol), 4- dibenzofuran boronic acid (8.5g, 70 mol), tetrakis (triphenylphosphine) palladium (1.36 g, 0.12 mmol), potassium carbonate (16.2 g, 117.3mmol) and the mixture of toluene 100 mL, 110mL of tetrahydrofuran, the water was added 40 mL. The temperature of the reactor temperature was raised to 80 degrees and stirred overnight. When the reaction is finished the temperature of the reactor was lowered to room temperature, extracted with ethyl acetate and the organic layer was separated. The organic layer was concentrated under reduced pressure and separated by column chromatography to give the intermediate 1-d. (15.0g, 67.1%)

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC Co.,Ltd; PARK, SOK BAE; SONG, JU MAN; LEE, YU RIM; KIM, HEE DAE; PARK, SANG WOO; JONG, GYUNG SOK; CHA, SUN WOOK; (60 pag.)KR2015/128583; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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 627-31-6, category: iodides-buliding-blocks

(b) Synthesis of 1-(4-nitro-phenyl)-cyclobutanecarboxylic acid methyl ester (4-Nitro-phenyl)-acetic acid methyl ester (15.21 g, 76.9 mmol) was dissolved in anhydrous DMF (80 mL) and allowed to stir until all solid dissolved. The solution was cooled to 0 C. with an ice bath. Sodium hydride (6.32 g, 153.8 mmol; 60% dispersion in oil) was added slowly and cautiously. The resulting mixture was allowed to warm to about 20-35 C. and was stirred for approximately 15 min. The solution was cooled again to 0 C. with an ice bath. 1,3-Diiodopropane (17.7 mL, 153.8 mmol) was added slowly and drop-wise, and the resulting solution was allowed to stir at 0 C. for about 30 min. The solution was warmed to about 20-35 C. and stirred at about 20-35 C. for about 1 h. The solution was cooled to 0 C. with an ice bath and quenched with H2O, maintaining 0 C. throughout the quenching process. The reaction mixture was extracted 3 times with dichloromethane. The combined organic layers were washed with water and brine; dried over sodium sulfate; filtered; and then concentrated under vacuum to give product. The material was purified by column chromatography (SiO2, 80:20 hexane: EtOAc) and gave the title compound as a yellow solid material (7.5 g, 41% yield).1H NMR (300 MHz, CDCl3, TMS) delta 1.87-2.19 (m, 2H), 2.48-2.58 (m, 2H), 2.86-2.95 (m, 2H), 3.67 (s, 3H), 7.43 to 7.48 (m, 2H), 8.17-8.21 (m, 2H).LC-MSD (ES+): (m/z) 236 [(M+H)+, 100].

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; Dr. Reddy’s Laboratories Ltd.; US2010/144722; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 5100-98-1, name is 3-Chloro-2-iodotoluene, 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 5100-98-1, Quality Control of 3-Chloro-2-iodotoluene

General procedure: A mixture of 17 (200 mg, 0.369 mmol), 2-bromo-1-methoxy-3-methylbenzene(148 mg, 0.737 mmol), Pd(OAc)2 (8.3 mg, 0.037 mmol), 2-dicyclohexylphosphino-2?,6?-di-isopropoxy-1,1?-biphenyl (34.4 mg,0.074 mmol), and Cs2CO3 (360 mg, 1.11 mmol) in toluene (7.5 ml) and water (1.5 ml) was stirred at 80 ¡ãC for 25 h. Then, water was added tothe reaction mixture, and the product was extracted with AcOEt. Theorganic layer was successively washed with water and brine, dried overanhydrous Na2SO4 and concentrated in vacuo. The residue was purifiedby silica gel column chromatography (hexane/AcOEt=40/60 to 10/90) to give the title compound as a white solid (43 mg, 21percent).

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

Reference:
Article; Murafuji, Hidenobu; Sugawara, Hajime; Goto, Megumi; Oyama, Yoshiaki; Sakai, Hiroki; Imajo, Seiichi; Tomoo, Toshiyuki; Muto, Tsuyoshi; Bioorganic and Medicinal Chemistry; vol. 26; 12; (2018); p. 3639 – 3653;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 702641-04-1, The chemical industry reduces the impact on the environment during synthesis 702641-04-1, name is 2-Iodo-5-(trifluoromethyl)benzoic acid, I believe this compound will play a more active role in future production and life.

A mixture of 2-iodo-5-(trifluoromethyl)benzoic acid (0.79 g, 2.5 mmol), 3-(trifluoromethyl)bicyclo[1.1.1]pentan-1-amine hydrochloride (0.52 g, 2.8 mmol), and O-(benzotriazol-1-yl)-N,N,N?,N?-tetramethyluronium tetrafluoroborate (TBTU, 0.88 g, 2.75 mmol) in dichloromethane (15 mL) was treated with N,N-diisopropylethylamine (1.3 mL, 7.5 mmol). The mixture was allowed to stir at room temperature overnight. The mixture was partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate solution. The latter was extracted three times with ethyl acetate. The combined organic extracts were washed successively with 10% aqueous hydrochloric acid and saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, filtered, and concentrated to dryness under reduced pressure to provide the desired intermediate. LCMS-ESI- (m/z): [M-H]- calcd 447.97; found 448.03

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-Iodo-5-(trifluoromethyl)benzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Gilead Sciences, Inc.; Farand, Julie; Kaplan, Joshua A.; Notte, Gregory; Olen, Casey Lockwood; Sangi, Michael; Sperandio, David; (115 pag.)US2019/359565; (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, category: iodides-buliding-blocks

Into a mixture of 2-bromo-1-(4-iodophenyl)ethanone (5g, 15.4 mmol) and (S)-1-(tert-butoxycarbonyl)pyrrolidine-2-carboxylic acid (3.48g, 16.1 mmol) in acetonitrile (40 mL) was added diisopropylethylamine (2.4 mL, 17 mmol). The resulting mixture was stirred at rt for 3 hours before being partitioned between EtOAc and aqueous NaHCO3. The organic phase was separated, dried (Na2SO4) and concentrated to afford a brown oil. It was purified by flash column chromatography (silica, hexane-EtOAc) to give the desired product as light yellow oil (6.0 g, 86%). ESIMS m/z=481.94 [M+Na]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-1-(4-iodophenyl)ethanone, and friends who are interested can also refer to it.

Reference:
Patent; Enanta Pharmaceuticals, Inc.; Qiu, Yao-Ling; Wang, Ce; Peng, Xiaowen; Ying, Lu; Or, Yat Sun; US2020/2314; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, 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. COA of Formula: C8H9I

Charged 1-iodo-3,4-dimethylbenzene (10.0 grams, 43.09 mmol, MW: 232.06), di(ethylene glycol) monohexylether (16.39 grams, 86.18 mmol, MW: 190.28), cesium carbonate, (21.23 grams, 64.60 mmol, MW: 328.5), 1,10-phenathroline (1.55 grams, 4.58 mmol, MW: 180.21), copper (1) iodide (0.447 grams, 2.29 mmol, MW: 195.01) and 50 milliliters of dry xylene in 350 milliliter three necked round bottom flask. The reaction mixture was heated with stirring at 140 C. for 24 hours under nitrogen. The resulting suspension was cooled to room temperature and filtered through celite and alumina. The low boiling (xylene) component removed by rotary evaporator and high boiling component by air bath oven at 180 C. under high vacuum. The residue was purified by flask chromatography on silica gel with hexane. The final yellow product was yielded 7.6 grams (60%). The product 13C NMR analysis suggests the formation of aryl ether product. 13C NMR (CDCl3): 157.42, 137.68, 130.34, 128.57, 116.37, 111.50, 71.64, 70.87, 70.15, 69.88, 67.46, 31.75, 29.68, 25.84, 22.66, 20.06, 18.79, 14.08.

The synthetic route of 4-Iodo-1,2-dimethylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ExxonMobil Research and Engineering Company; Patil, Abhimanyu O.; Bodige, Satish; (23 pag.)US2017/137735; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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 627-31-6, Application In Synthesis of 1,3-Diiodopropane(stabilized with Copper chip)

A THF solution (12 mL) of the above-mentioned colorless oily matter (153 mg, 0.45 mmol) was cooled to -40 C., and LDA (0.7 mL, 1.4 mmol) was then added. This was stirred at -40 C. for 0.5 hour. Thereafter 1,3-diiodopropane (0.26 mL, 2.3 mmol) was added thereto, which was then stirred at -40 C. for three hours. After that, a saturated ammonium chloride aqueous solution was added. Subsequently, the organic layer was separated and an aqueous layer was extracted with ethyl acetate. The mixed organic layer was washed with saturated saline, dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The crude extract thus obtained was purified using column chromatography (n-hexane:ethyl acetate=4:1). Thus MI-22 (22 mg, 21%) was obtained as a colorless oily matter. The respective data of the infrared (IR) absorption spectrum, the nuclear magnetic resonance (1H, 13C-NMR) spectrum, and the mass spectrometry (FAB) of the MI-22 are indicated below: IR (KBr) 3416, 2855, 1614 cm-1; 1H NMR (CDCl3, 300 MHz): delta 0.88 (6H, t, J=6.4 Hz), 1.09 (6H, t, J=7.2 Hz), 1.14 (6H, t, J=7.2 Hz), 1.20-1.38 (48H, m), 1.50-1.62 (2H, m), 1.98-2.03 (8H, m), 2.42-2.52 (2H, m), 3.31 (4H, q, J=7.2 Hz), 3.36 (4H, q, J=7.2 Hz), 5.32-5.35 (4H, m); 13C NMR (CDCl3, 300 MHz): delta 12.9, 13.9, 14.8, 22.5 (2C), 27.0 (2C), 27.4, 29.0 (3C), 29.3, 29.6 (2C), 31.7 (2C), 33.3, 33.5, 40.2, 41.0, 41.6, 129.5, 129.7, 175.1; and LRMS (FAB) m/z 716 (MH+). HRMS (FAB) calcd for C47H91N2O2, 715.7081; found, 715.7078.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Diiodopropane(stabilized with Copper chip), and friends who are interested can also refer to it.

Reference:
Patent; Nojima, Hiroshi; Kita, Yasuyuki; US2008/89924; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 34683-73-3, 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. 34683-73-3, name is 1-Chloro-6-iodohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of 2,2′-bithiophene (10.0 g, 60.24 mmol) in anhydrous THF (150 ml) was added n-butyllithium (2.5 M in hexanes, 20.0 ml, 50.0 mmol) dropwise at -78 C under nitrogen. After complete addition, the mixture was allowed to warm to room temperature, with stirring, over 2 h, followed by the addition of 1- chloro-6-iodohexane (14.55 g, 50.0 mmol). The resultant mixture was stirred overnight at room temperature. The reaction was quenched with sat. aq. NH4CI, and the reaction mixture was extracted with ethyl acetate (3 x 100 ml). The combined organic extracts were washed with water, brine, and dried over sodium sulphate. The solvent was removed under reduced pressure and the residue was purified by column chromatography on silica, eluting with petroleum ether, to give 5-(6-chlorohexyl)-2,2′-bithiophene as a white solid (7.73 g, 54 %). ?H NMR (300 MHz, CDC13): 8 (ppm) 7.14 (d, J = 5.3 Hz, 1.3 Hz, 1 H, Ar- H), 7.08 (dd, J = 3.5 Hz, 1.1 Hz, 1 H, Ar-H), 6.97 (m, 2H, Ar-H), 6.66 (d, J = 3.5 Hz, 1 H, Ar-H), 3.51 (d, J = 6.6 Hz, 2H, CICH2), 2.78 (t, J = 7.1 Hz 2H, ArCH2), 1.61-1.81 (m, 4H, CH2), 1.35-1.51 (m, 4H, CH2); MS (m/e): 282 (M+, 2 %), 166 (8), 123 (39), 110 (22), 97 (100)

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-Chloro-6-iodohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK PATENT GMBH; WO2005/121150; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, 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 608-28-6, Product Details of 608-28-6

To a test tube containing a magnetic bar was added aryl halide (1.0 mmol), CuCl2 (13.4 mg, 0.1 mmol), KOH (336 mg, 6.0 mmol), ethylene glycol(12 muL, 0.2 mmol), and DMSO/H2O (1.0 mL/0.5 mL). After flushing with argon, the mixture was stirred in a preheated oil bath at 120 C for 24 h. After cooled to ambient temperature, the reaction mixture was distributed in aqueous HCl (5 %) and ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous MgSO4, and concentrated under vacuum. The crude product was further purified by column chromatography (EtOAc/n-Hexane) to provide the phenols.

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; Kim, Jihye; Battsengel, Oyunsaikhan; Liu, Yajun; Chae, Junghyun; Bulletin of the Korean Chemical Society; vol. 36; 12; (2015); p. 2833 – 2840;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 689260-53-5, These common heterocyclic compound, 689260-53-5, name is 2-Bromo-5-iodo-1,3-dimethylbenzene, 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.

In a microwave vial 2-bromo-5-iodo-1 ,3-dimethylbenzene (1 g) and 5-(4,4,5,5- tetramethyl-1 ,3,2-dioxaborolan-2-yl)pyrimidine (665 mg) are suspended in N,N- dimethylformamide (15 mL) and Na2CO3 (4 mL of a 2 M aqueous solution). The mixture is purged for 5 minutes with argon. [1 ,1 ‘-Bis(diphenylphosphino)-ferrocene]- dichloropalladium dichloromethane complex (85 mg) is added, the vial is sealed and the mixture is stirred at 60C for 3 hours. After cooling to room temperature the mixture is Partitioned between water and ethyl acetate. The aqueous phase is extracted with ethyl acetate and the combined organic phases are washed with brine. Then the organ ic phase is dried (MgSO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 80:20?50:50) to give the title compound. Yield: 446 mg; LC (method 9): tR = 1 .05 min; Mass spectrum (EST): m/z = 263 [M+H]+.

The synthetic route of 689260-53-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ECKHARDT, Matthias; FRATTINI, Sara; HAMPRECHT, Dieter; HIMMELSBACH, Frank; LANGKOPF, Elke; LINGARD, Iain; PETERS, Stefan; WAGNER, Holger; WO2013/144097; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com