Tag: M.W=300-400

112671-42-8, 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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows.

mixture of compound 71 (6.5 g, 19.8 mmol) and Fe (4.98 g, 89.2 mmol) inCH3COOH (30 mL) and CH3CH2OH (30 mL), was refluxed for 1.5 hours. The mixture was cooled to room temperature and after addition of saturated NaHC03 (aq.), extracted with ethyl acetate (3 x 150 mL).The combined organic layer was separated, dried over Na2S04 and the solvent was removed in vacuo, resulting in compound 72 (5.9 g). Method A2; Rt: 1.17 min. m/z=: 299.6 (M+H)+ Exact mass: 298.9

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; TIBOTEC PHARMACEUTICALS; VANDYCK, Koen; VERSCHUEREN, Wim Gaston; RABOISSON, Pierre Jean-Marie Bernard; WO2012/13643; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

121554-10-7, A common heterocyclic compound, 121554-10-7, name is 5-Bromo-2-iodobenzonitrile, molecular formula is C7H3BrIN, 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.

EXAMPLE 112a Preparation of intermediate 5-bromo-2-iodo-benzaldehyde To a solution of 5-bromo-2-iodo-benzomitrile (1.54 g, 5 mmol) in DCM (15 mL) was added a solution of DIBALH (6 mL, 6 mmol) dropwise at 0 C. After the addition, the reaction mixture was warmed to r.t. and stirred for 2 h. Then the mixture was poured into 20 g of ice and 20 mL of 1N HCl, filtered and extracted by DCM (40 mL), washed with aqueous sodium bicarbonate, dried over MgSO4 and concentrated to give crude product (Yield: 1.2 g).

The synthetic route of 121554-10-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ding, Qingjie; Jiang, Nan; Yang, Song; Zhang, Jing; Zhang, Zhuming; US2009/156610; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

61203-48-3, The chemical industry reduces the impact on the environment during synthesis 61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic acid, I believe this compound will play a more active role in future production and life.

[C.] [N- (8-NITROQUINOLIN-4-YL)-N- (N, N-DIMETHYLAMINOETHYL)-2-IODO-5,] 6- dimethoxybenzamide (8a). Oxalyl chloride (762 mg, 6.0 mmol) was added to a solution of 3,4-dimethoxy-6-iodobenzoic acid (570 mg, 1.85 mmol) in anhydrous methylene chloride (20 mL), and the stirred mixture was refluxed for 3 hours. The mixture was then concentrated to dryness under reduced pressure. The acid chloride was redissolved in 20 mL of anhydrous methylene chloride, and this solution was added to a solution of 7a (400 mg, 1.54 mmol) and triethylamine (1.14 g, 11.3 mmol) in methylene chloride (20 mL), and the resulting mixture was stirred at reflux overnight. The reaction mix was cooled and washed with saturated sodium bicarbonate (3 x 75 mL), and extracted with 5 % aqueous [HC1] (4 x 100 mL). The combined aqueous extracts were basified with 30% [NAOH] and then extracted with chloroform (3 x 100 mL). Combined organic extracts were then dried [(MGS04)] and evaporated to give 722 mg of the amide, in 85 % yield [; IH] NMR [(CDC13)] 6 2.30 (s, 6H), 2.69 (m, 2H), 3.32 (s, 3H), 3.74 (s, 3H), 3.95 (m, 1H), 4.57 (m, 1H), 6.41 (s, 1H), 7.02 (s, 1H), 7.75 (m, 2H), 8.05 (d, 1H, [J=6.] 6), 8.44 (d, 1H, [J=8.] 4), 8.95 (d, 1H, [J=4.] 4) [; 13C NMR] [(CDC13)] [5] 45.4, 47.3, 55.7, 56.1, 56.5, 82.7, 110.7, 121.9, 123.3, 124.0, 126.1, 126.9, 127.2, 133.1, 140.9, 147.4, 148.4, 149.0, 150.1, 153.0, 169.9 ; IR (CHC13) 1362,1536, 1655.

The chemical industry reduces the impact on the environment during synthesis 2-Iodo-4,5-dimethoxybenzoic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; RUTGERS, THE STATE UNIVERSITY; LAVOIE, Edmond, J.; RUCHELMAN, Alexander, L.; LIU, Leroy, F.; WO2004/14906; (2004); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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.

Intermediate Ml-a (5. lg, 18.4 mmol) and 2_p_5_ nitrobenzene (15.3 g, 46.7 mmol), tert-butanol sodium (7. lg, 74.4 mmol), toluene 100 mL, nitrogen Protection, 0.3g Pd2 (dba) 3, tri-tert-butylphosphine (20ml, 10% toluene solution), start stirring, heat to 100 C reflux, reaction 12h, the reaction liquid is washed, the organic phase is concentrated, passed through the silica gel column, rinse The oil was petroleum ether: ethyl acetate = 50:1, and the eluent was concentrated to give intermediate Ml-b (9.2 g, yield: 7.39 %).

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; Beijing Dingcai Technology Co., Ltd.; Gu’an Dingcai Technology Co., Ltd.; Fan Hongtao; Zhang Yaguang; Zhang Xianghui; Ren Xueyan; (28 pag.)CN108341826; (2018); A;,
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 25252-00-0 as follows. 25252-00-0

To commercially available 2-bromo-5-iodobenzoic acid (76.5 mmol, 25 g), hydroxybenzotriazole (HOBt, 76. 5mmol, 10.4 g), triethylamine (TEA, 153 mmol, 21.3 mL) and ammonium chloride (84.1 mmol, 4.50 g), is added DMF (anhydrous, 300 mL). After dissolution of solids by stirring, 1- [3- (Dimethylamino) propyl]-3- ethylcarbodiimide hydrochloride (EDC-HCI, 84.1 mmol, 16.08 g) is added. Stirring continues with the reaction capped for 16 hours. The reaction is concentrated to half the original volume via roto-evaporation, then 1 L ethyl acetate is added and the subsequent solution is washed once with 1 M HCI (300 mL), then once with saturated NaHCO3 (300 mL), then twice with H20, and then once with saturated NaCI (100 mL). A white solid resulted on drying the ethyl acetate phase with MgS04, filtering through celite, and evaporation of volitiles. LCMS : Method [11] : Retention time at 220nm detection is 1.51 minutes and [M = 1] + = 325.8. LCMS shows nearly quantitative product (i) at >95% purity.

According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; WO2005/87751; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

364-11-4, A common compound: 364-11-4, name is 1-Bromo-4-iodo-2-(trifluoromethyl)benzene, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

To a solution of 1-bromo-4-iodo-2-(trifluoromethyl)benzene (246 mg, 0.701 mmol) in 1.4 mL of Et2O (C=0.5M) was added dropwise a 1.6M solution of BuLi in hexane (460muIota., 1.05 eq) at -78C. After 15 min of stirring, benzaldehyde (86muIota., 1.2 eq) was slowly added. The mixture was stirred for 4h at -75 C and then, hydrolyzed with water and with a 1M HC1 solution to acidify. The layers were separated. The aqueous layer was extracted with DCM (3>< 10mL). The combined organics were washed with brine, dried over MgSO4, filtered and solvents were removed in vacuo. The crude residue was purified by silica gel flash chromatography (cyclohexane/AcOEt 93:7 to 90: 10) to afford the desired product in 76% yield (176 mg) as an uncoloured oil. 1H NMR (300 MHz, CDC13) delta 7.76 (d, J = 2.2 Hz, 1H), 7.65 (d, J = 8.3 Hz, 1H), 7.41 - 7.27 (m, 6H), 5.81 (s, 1H), 2.36 (s, OH); 13C NMR (75 MHz, CDCI3) delta 143.5 (C), 142.8 (C), 135.1 (d, J = 2.0 Hz, CH), 131.0 (CH), 130.2 (q, J = 31.3 Hz, C), 129.0 (CH), 128.5 (CH), 126.7 (CH), 125.9 (q, J = 5.4 Hz, CH), 123.0 (q, J = 273.6 Hz, C), 1 18.9 (q, J = 2.0 Hz, C), 75.4 (CH); MS (ESI) m/z : 313.0, 315.0 [M-OH, 79Br, 81Br]+; 348.0, 350.0 [M+NH4, 79Br, 81Br]+; 680.0 [2M+NH4, 79Br, 81Br]+. 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-Bromo-4-iodo-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see. Reference:
Patent; UNIVERSITA’ DEGLI STUDI DI MILANO – BICOCCA; UNIVERSITE DE GENEVE; UNIVERSITE CLAUDE BERNARD – LYON 1; GAMBACORTI-PASSERINI, Carlo; MOLOGNI, Luca; SCAPOZZA, Leonardo; BISSON, William; AHMED, Shaheen; GOEKJIAN, Peter; TARDY, Sebastien; ORSATO, Alexandre; GUEYRARD, David; BENOIT, Joseph; WO2013/167730; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 915095-86-2, name is (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, 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 915095-86-2, 915095-86-2

5-Iodo-2-chloro-4′-fluorobenzophenone (V-2) (18.5 g, 0.051 mol) was dissolved in 50 ml of tetrahydrofuran solutionThen, (5)-3_light-based tetrahydrofuran (4.9 g, 0.056 mol) was added and stirred, and finally a solution of potassium t-butoxide (6.9 g, 0.061 mol) dissolved in 30 ml of tetrahydrofuran was added dropwise, and the temperature was controlled at 16-25 ¡ã C. After the addition was completed, the reaction was stirred at 20 ¡ã C for 1 hour, and the reaction was almost complete by TLC, and the purified water was slowly added and stirred for 30 min.The solution was separated and the organic phase was dried. After column chromatography, 14. lg (64.3percent) of solid was obtained.

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-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Huarun Shuang He Pharmaceutical Co., Ltd.; Zhai Jianguo; He Yang; Zhu Yingjie; Zhou Yisui; Ma Hongmin; Song Meng; (46 pag.)CN108218928; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

25252-00-0, Adding a certain compound to certain chemical reactions, such as: 25252-00-0, name is 2-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 25252-00-0.

General procedure: To a solution of 0.5 g compound 3(0.10 mol) in 3 ml DMF, 3.3 mg (0.01 mol) of copper iodide, 0.57 gcesium carbonate (0.1 mol), 20 mg (0.01 mol) Tetrakis (triphenylphosphine)palladium(0) was added under nitrogen atomophere. Then arylhalide (4-12) 0.11 mol was added under nitrogen atm, the mass wasstirred for 8 hrs at 75 C under nitrogen atm. Reaction was completed asindicated by TLC and the reaction mass was filtered through cellite bed,washed the bed with ethyl acetate (10 ml). The product layer (Ethylacetate layer)was then washed with water 10.0 ml, sodium bi sulphite10 ml followed by saturated sodium chloride solution (5.0 ml) and driedover (Na2SO4). The solvent was distilled off and the resulting productwas purified by column chromatography using ethyl acetate and nhexaneto get the pure product (4a-l). Yield observed was around85-90% for all the derivatives.

According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Thangarasu; Thamarai Selvi; Manikandan; Bioorganic Chemistry; vol. 81; (2018); p. 468 – 480;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, Name is 1,4-Diiodobutane, 628-21-7, 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.

5-Bromo-2- (4-methoxybenzyl) -7-methyliso-1-one at 0 C(3.0 grams, 8.7 moles)N, N-dimethylformamide (30mL)To the solution was added sodium hydride (1.043 g, 43.5 moles).The reaction solution was stirred at room temperature for 10 minutes.Then add 1,5-diiodopentane (3.493 g, 11.3 mol),The reaction solution was stirred at room temperature for 4 hours.After the reaction was monitored by TLC, the reaction was quenched with saturated ammonium chloride solution, and the mixture was extracted with ethyl acetate (100 mL x 2). The organic layers were combined, dried over anhydrous sodium sulfate, filtered and concentrated. The crude product was purified by flash column chromatography (petroleum ether / ethyl acetate = 1/1) to give the product in the form of an oil (1.97 hag, yield 56.8%).

Statistics shows that 1,4-Diiodobutane is playing an increasingly important role. we look forward to future research findings about 628-21-7.

Reference:
Patent; Nuowosida Pharmaceutical Co., Ltd.; Li Bing; (67 pag.)CN110256432; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

112671-42-8, 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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The starting material, phenylboronic acid (76.84g, 630.2mmol) was dissolved in a THF (2780ml) in a round bottom flask, 4-bromo-1-iodo-2-nitrobenzene (309.96g, 945.3mmol), Pd (PPh3) 4 ( 36.41g, 31.5mmol), was added K2CO3 (261.3g, 1890.6mmol), water (1390ml) and the resulting mixture was stirred at 80 . Once the reaction is complete, the organic layer extracted with water and CH2Cl2After the dried over MgSO4 and concentrated to a silicagel column and the resulting compound was recrystallized 122.68g product (yield: 70%)It was obtained.

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

Reference:
Patent; Duksan Neolux Co, Ltd.; Moon, Song Yoon; Lee, Son Hui; Park, Jong Cheol; Kim, Dae Song; Lee, Bom Song; Park, Song Jae; (89 pag.)KR101550768; (2015); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com