Tag: M.W=300-400

Application of 180624-08-2, 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. 180624-08-2, name is 4-Bromo-2-iodo-6-nitroaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of Intermediate 1A (4.5 g, 13.12 mmol) in EtOH (80 mL) was added concentrated HCl (5.47 mL, 65.6 mmol), followed by tin(II)chloride dihydrate (11.84 g, 52.5 mmol). The reaction mixture was stirred at 60C overnight. After cooled to room temperature, it was treated with an ice-cold 4.0 N NaOH (18 mL) and EtOAc/water. After stirring for 1 min, the white solid was removed by filtration. The filtrate was separated, the organic layer was collected, washed with brine and dried over sodium sulfate. After evaporation of solvent, the crude product was dissolved in a small amount of chloroform and charged to an 80 g silica gel cartridge which was eluted with 5% for 3 min, then a 12 min gradient from 5% to 50%; The desired fractions were combined and concentrated to give Intermediate 1B (3.3 g, 10.55 mmol, 80% yield) as a pale brown solid; 1H NMR (500 MHz, chloroform-d) delta 7.33(d, J=2.2 Hz, 1H), 6.83(d, J=1.9 Hz, 1H), 3.81(br s, 2H), 3.54(br s, 2H); LC-MS: method A, RT=1.82 min; MS (ESI) m/z: 312.8 and 313.8 (M+H)+;

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-2-iodo-6-nitroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ZHANG, Xiaojun; ZHENG, Xiaofan; CHUPAK, Louis S.; (102 pag.)WO2017/19828; (2017); 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 51839-15-7 as follows. Safety of Dimethyl 5-iodoisophthalate

Dimethyl 5-iodoisophthalate(2.9 g, 8.9 mmol) and THF (50 mL) was cooled to -20 C.,A THF solution (about 14% by mass, 8.4 mL, 8.1 mmol) of isopropyl magnesium chloride-lithium chloride complex was added dropwise.The obtained mixture was stirred at -20 C. for 1 hour,Copper (I) bromide-dimethyl sulfide complex (1.9 g, 9.1 mmol) was added.The resulting mixture was heated to 30 C. and a solution of C60 fullerene (0.72 g, 1.0 mmol) in ODCB (50 mL) was added.The obtained mixture was stirred at 60 C. for 4 hours,Saturated aqueous ammonium chloride solution (1 mL) was added.The resulting mixture was filtered and the volume of the solution was reduced with a rotary evaporator.By adding methanol to the obtained mixture,As a reddish brown solid substance, Compound 7 (C7)(1.5 g, 0.90 mmol,Yield: 90%) was precipitated

According to the analysis of related databases, 51839-15-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Showa Denko; Watanabe, Kentaro; Ueda, Yoshiyuki; Hanawa, Kenzo; (53 pag.)JP2018/203686; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 672-57-1, 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. 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 5:- Preparation of 7-(2-chloro-5-trifluoromethyl-phenylethynyl)-2-(2,6-dibromo- phenyl)-4,4-dimethyl-l,4-dihydro-chromeno[3,4-d]imidazole:-The mixture of 2-(2,6-dibromo-phenyl)-7-ethynyl-4,4-dimethyl-l,4-dihydro- chromeno[3,4-d]imidazole (0.500 g, 109 mol), dichloro bis (triphenyl phosphine)palladium (II) (0.022 g, 0.0327 mol), tetra butyl ammonium fluoride (0.855 g, 3.27 mol) and l-chloro-2-iodo-4-trifluoromethyl-benzene (0.501 g, 1.63 mol) was heated at 80-90C for 2-3 hours. The reaction mass was quenched in water and extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford desired product (0.230 g). ‘HNMR (DMSO- 6): delta 1.65 (s, 6H), 7.09-7.11 (m, 1H), 7.21-7.24 (m, 1H), 7.38-7.44 (m, 1H), 7.52 (m, 1H), 7.77-7.87 (m, 4H), 8.08 (s, 1H), 13.09 (s, 1H).

The synthetic route of 1-Chloro-2-iodo-4-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; GHARAT, Laxmikant Atmaram; GAJERA, Jitendra Maganbhai; NARAYANA, Lakshminarayana; KHAIRATKAR-JOSHI, Neelima; KATTIGE, Vidya Ganapati; WO2012/110860; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 51839-15-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 51839-15-7 name is Dimethyl 5-iodoisophthalate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: A 15 mL heavy walled pressure tube sealable with a gasketed Teflon screwcap was charged with a diaryl iodonium triflate (0.2 mmol, 1 equiv), an aryl iodide (1.0 mmol, 5 equiv.), and 1,2-dicholoroethane (2 mL, 0.1 M iodonium triflate concentration). The tube was sealed (Teflon screw cap) and immersed in an oil bath maintained at 80 C. 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).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Dimethyl 5-iodoisophthalate, and friends who are interested can also refer to it.

Reference:
Article; Racicot, Leanne; Ciufolini, Marco A.; Tetrahedron; vol. 73; 50; (2017); p. 7067 – 7072;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route 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

Application of 112671-42-8,Some common heterocyclic compound, 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, molecular formula is C6H3BrINO2, 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.

(1) In the reaction bottle, add N-phenylcarbazole-4-boronic acid (100mmol), 2-iodo-5-bromonitrobenzene (100mmol), 0.9g (0.785mmol, 0.5%) tetratriphenylphosphine Palladium, toluene 500mL, ethanol 200mL, water 200mL, and potassium carbonate 40g (300mmol), react at 100 C for 8h; after the reaction is complete, stop the reaction; cool to room temperature, separate the organic phase, concentrate, silica gel column chromatography to obtain yellow powder M1;

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Bromo-1-iodo-2-nitrobenzene, its application will become more common.

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (24 pag.)CN110734446; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, A new synthetic method of this compound is introduced below., Recommanded Product: 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

A mixture of (S)-N- [(4,5 -dimethoxybenzocyclobut- 1 -yl)methyl] -N-(methyl)amine hydrochloride (lOOg) and d.imethyl formamide (400mL) was stirred for about 5mm and potassium carbonate (178.46g) was added to it. The reaction mixture was stirred forabout lh at about room temperature. The reaction mixture was cooled to about 5C to about 10C. 7, 8-dimethoxy-3 -[3 -iodopropyl] – 1,3 -dihydro-2H-3 -benzazepin-2-one (3 6g) prepared as in Example 8, was added to the stirred reaction mixture. The reaction mixture was stirred for about 4h at about 20C to about 25C. The reaction mixture was quenched into chiHed demineralized water at about 5C to about 10C. The reaction mixture wasacidified to pH of about I to about 2 using concentrated hydrochloric acid and ethyl acetate was added to it. The reaction mixture was stirred and the two layers were separated. The aqueous layer was basified to pH of about 8 to about 9.5 using 20-25% aqueous ammonia solution and ethyl acetate was added to it. The reaction mixture was stirred and the two layers were separated. The organic layer was washed withdemineralized water and concentrated under reduce pressure at about below 55C.Yield: 75%; HPLC purity: > 96%

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; GLENMARK PHARMACEUTICALS LIMITED; GLENMARK GENERICS LIMITED; BHIRUD, Shekhar Bhaskar; BHUSHAN, Kumar Hari; ZOPE, Sunil Sudhakar; PATIL, Dipak Vinayak; DHEBADE, Pramod Amrutrao; CHAND, Prem; WO2014/102827; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 16355-92-3, The chemical industry reduces the impact on the environment during synthesis 16355-92-3, name is 1,10-Diiododecane, I believe this compound will play a more active role in future production and life.

2-Picoline (0.30 mL, 3.1 mmol) and 1,10-diiododecane (13.0 g, 33 mmol) were dissolved in acetone (20 mL) with a 50 mL flask equipped with a condenser. The solution was heated to reflux at 60C for 4 days. The solution was dropped into hexane (300 mL), and then a yellow precipitate was obtained. The precipitate was recovered and dried to obtain the product 4 as yellow powder (yield 1.3 g, 87%). 1H NMR (500MHz, DMSO-d6): delta 8.96 (d, J=5.1Hz, 1H), 8.44 (t, J=7.8Hz, 1H), 8.02 (d, J=7.9Hz, 1H), 7.94 (t, J=6.8Hz,1H), 4.51 (t, J=7.8Hz, 2H), 3.25 (t, J=6.8Hz, 2H), 2.82 (s, 3H), 1.85-1.79 (m, 2H), 1.75-1.69 (m, 2H), 1.36-1.22 (m, 12H).

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, 1,10-Diiododecane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Hashidzume, Akihito; Kuse, Akihiro; Oshikiri, Tomoya; Adachi, Seiji; Yamaguchi, Hiroyasu; Harada, Akira; Tetrahedron; vol. 73; 33; (2017); p. 4988 – 4993;,
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 34270-90-1 as follows. Computed Properties of C4H8I2O

A mixture of compound 1 (1 mmol), 1-iodo-2-(2-iodoethoxy)ethane (1 mmol) and anhydrouspotassium carbonate (140 mg, 1 mmol) in anhydrous acetonitrile (10 mL) was heated under reflux for1 h and then quenched with water (5 mL). Product 47 was extracted with ethyl acetate and purified ona chromatotron eluting with dichloromethane/methanol (8:2).Yield 66%; m.p. >200 C (decomp.); 1H-NMR (DMSO-d6): delta 8.55 (m, 1H), 8.46 (d, J = 5.2 Hz, 1H), 7.83(m, 1H), 7.10 (m, 2H), 4.13 (m, 4H), 3.98 (m, 4H), 3.74 (m, 4H), 3.67 (m, 4H). HR-MS (ESI). Calcd forC16H21N4O2 (M+): m/z 301.1665. Found: m/z 301.1650. Anal. Calcd for C16H21N4IO2: C, 44.87; H, 4.94;N, 13.08. Found: C, 44.97; H, 5.09; N, 12.69.

According to the analysis of related databases, 34270-90-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Strekowski, Lucjan; Saczewski, Jaros?aw; Raux, Elizabeth A.; Fernando, Nilmi T.; Klenc, Jeff; Paranjpe, Shirish; Raszkiewicz, Aldona; Blake, Ava L.; Ehalt, Adam J.; Barnes, Samuel; Baranowski, Timothy C.; Sullivan, Shannon M.; Sata?a, Grzegorz; Bojarski, Andrzej J.; Molecules; vol. 21; 4; (2016);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, 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 755027-18-0, category: iodides-buliding-blocks

Step 4: l-Bromo-4-iodo-2-methoxybenzene (50 g, 160 mmol) was suspended in dichloromethane (75 mL) at -10 C. 1 N BBr3 in CH2Cl2 (250 mL, 250 mmol) was cannulated in over 30 minutes, with the internal temperature remaining below 0 C throughout the addition. After the addition, the mixture was stirred at 0C for 1 h, and then at room temperature for an additional 16 h. The mixture was cooled in an ice bath. 10% Aqueous Na2C03 (250 mL) was added in portions. The mixture was then partitioned between H20 and dichloromethane. The dichloromethane layer was dried over MgSCU and then filtered. 2-Bromo-5-iodophenol (46 g, 96%) was obtained from the filtrate as a pinkish- white solid. (1119) 1H NMR (acetone-< d: 9.24 (br s, 1H), 7.38 (d, J= 2 Hz, 1H), 7.31 (d, J= 8.5 Hz, 1H), 7.17 (dd, J= 8.5 Hz, 2 Hz, 1H). 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; PTC THERAPEUTICS, INC.; SYDORENKO, Nadiya; ALAM, Md Rauful; ARNOLD, Michael A.; BABU, Suresh; BHATTACHARYYA, Anuradha; CHEN, Guangming; GERASYUTO, Aleksey I.; KARP, Gary Mitchell; KASSICK, Andrew J.; MAZZOTTI, Anthony R.; MOON, Young-Choon; NARASIMHAN, Jana; PATEL, Jigar; TURPOFF, Anthony; WOLL, Matthew G.; YAN, Wuming; ZHANG, Nanjing; (0 pag.)WO2020/5873; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com