Tag: M.W=300-400

Reference of 188815-32-9, 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. 188815-32-9, name is 3-Bromo-5-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 4.539; 3-(5 -Chloropyridin-2-ylV 5-f 1 -hydroxy- 1 -methylethylVN- U 1 R )- 1 – 1 -oxido-6- f trifluoromethyl)pyridin-3 -yl] ethyl I benzamide; Step A: methyl 3-bromo-5-iodobenzoate; To a suspension of 3-bromo-5-iodobenzoic acid (993 g, 3.04 mol) in methanol (6.0 L) was added hydrochloric acid (37%; 20.0 mL, 244 mmol). The mixture was heated to 70 0C. After 72 h, the mixture was cooled to ambient temperature. Dichloromethane (2.5 L) was added and the mixture was partially concentrated. The suspension was filtered and the filtered cake was washed with cold methanol to give the title compound as a white solid (846 g)-

The chemical industry reduces the impact on the environment during synthesis 3-Bromo-5-iodobenzoic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; MERCK & CO., INC.; WO2009/58298; (2009); A1;,
Iodide – Wikipedia,
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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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, A new synthetic method of this compound is introduced below., name: 2-Bromo-1-(4-iodophenyl)ethanone

General procedure: To a mixture of olefin (0.5 mmol) and tween-80 (30 mL) in water (3 mL) was added DBH (214.5 mg, 0.75 mmol) at room temperature, and the mixture was stirred under the conditions as indicated in Table 1. After cooling to room temperature and removal of solvent under reduced pressure, EtOH (3 mL), thiourea (57.1 mg, 0.75 mmol) (or 0.75 mmol of N-methylthiourea/N-phenethylthiourea) were added to the mixture, and the obtained mixture was stirred for 2 h at 80 C. The mixture was diluted with ethyl acetate (60 mL). The organic phase was washed with brine (10mL x 3) and dried over Na2SO4. After concentrated under reduced pressure, the residue was purified by preparative thin layer chromatography to afford the corresponding 2-aminothiazoles.

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:
Article; Ma, Chunhua; Miao, Yuqi; Zhao, Minghao; Wu, Ping; Zhou, Jianglu; Li, Zhi; Xie, Xilei; Zhang, Wei; Tetrahedron; vol. 74; 27; (2018); p. 3602 – 3607;,
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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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, A new synthetic method of this compound is introduced below., Product Details of 31827-94-8

A 1 L round bottom flask equipped with a mechanical stirrer, thermocouple, and a reflux condenser was charged with 2′-bromo-4-iodoacetophenone (44.0 g, 0.135 mol), potassium acetate (19.9 g, 0.203 mol), benzyl triethylammonium chloride (1.5 g, 0.007 mol) and 1,2-dichloroethane (425 mL). The reaction mixture stirred at 70 C. for 4 hours then was cooled to 25 C. Water (250 mL) was added and the contents were shaken in a separatory funnel. The dichloroethane layer was separated and was washed with aq. saturated sodium bicarbonate (200 mL) and brine (100 mL). The dichloroethane was dried over sodium sulfate, filtered, and the solvents were removed under reduced pressure to give product as a tan solid (41.2 g, 97% yield): mp 103-107 C.

The synthetic route of 31827-94-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tisdell, Francis Eugene; Bis, Scott Jerome; Hedge, Vidyadhar Babu; Martin, Timothy Patrick; Perreault, Denise Marie; Yap, Maurice Chee Hoong; Guenthenspberger, Katherine Anne; Dripps, James Edwin; Gifford, James Michael; Schoonover, Joe Raymond; Karr, Laura Lee; Dintenfass, Leonard Paul; Neese, Paul Allen; US2004/6108; (2004); A1;,
Iodide – Wikipedia,
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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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 328-73-4

Magnesium (230 mg) was added to 3,5-bis (trifluoromethyl) phenyl iodide (3.0 g, 8.8 mmol) in tetrahydrofuran (THF, 80 ml) and stirred for 1-5 hours.The temperature was lowered to -20 ° C and 3.0 g of DMTr-protected propylene oxide (8 mmol) in THF (10 ml) was added. Two hours after the reaction was returned to room temperature for 8 hours. Workup and purification by column chromatography gave 3.73 g of compound 7 (79percent).

The synthetic route of 328-73-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Shanghai Organic Chemistry Institute; Wang Ruowen; Qing Fengling; (27 pag.)CN103880877; (2017); B;,
Iodide – Wikipedia,
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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. 199850-56-1, name is Methyl 2-amino-4-chloro-5-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: Methyl 2-amino-4-chloro-5-iodobenzoate

Intermediate 55 : Methyl 4-chloro-2-{[3-(ethyloxy)-3-oxopropanoyl1amino)-5-iodobenzoateTo a solution of methyl 2-amino-4-chloro-5-iodobenzoate (Intermediate 2) (8 g, 25.7 mmol) and pyridine (2.18 mL, 27 mmol) in dichloromethane (200 mL) was added ethyl 3-chloro-3- oxopropanoate (Aldrich, 3.45 mL, 27 mmol) and the reaction mixture was stirred overnight at room temperature. The reaction mixture was evaporated to dryness, diluted with ethyl acetate, washed successively with water and brine. The organic layer was then dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was triturated in pentane, filtered and dried to give the title compound methyl 4-chloro-2-{[3-(ethyloxy)-3- oxopropanoyl]amino}-5-iodobenzoate (8.24 g, 19.36 mmol, 75 % yield) as beige solid. LCMS: (M+H)+ = 426 ; Rt= 3.78 min.

According to the analysis of related databases, 199850-56-1, the application of this compound in the production field has become more and more popular.

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

Reference of 63131-30-6, 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 63131-30-6 as follows.

10 ml test tube reaction of adding 0.2mmol2 – (4-methoxyphenylamino) methyl acetate and 0.01mmol trifluoro methane sulfonic acid copper, in order to 3 ml acetonitrile as the reaction solvent, added under stirring 0.1mmol4-iodophenylamino Carbamoyl ethyl acetate, the (green) LED illumination the reaction solution 1h rear, turns on lathe does reaction solvent, after column separation, the obtained product is nuclear magnetism hydrogen spectrum carbon spectrum and mass spectrum is identified as 1-ethyl 4-methyl 2 – (4-iodo benzoyl) – 3 – ((4-methoxylphenyl) amino) succinate

According to the analysis of related databases, 63131-30-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Technical Institute of Physics and Chemistry of the Chinese Academy of Sciences; WU, LIZHU; GAO, XUEWANG; MENG, QINGYUAN; LEI, TAO; ZHONG, JIANJI; XIANG, MING; TONG, ZHENHE; (21 pag.)CN104230734; (2016); B;,
Iodide – Wikipedia,
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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, name: 2-Bromo-1-(4-iodophenyl)ethanone

General procedure: Sodium sulfite, sodium bicarbonate and sulfonyl chlorides in water were irradiated at 500 W for 20 min in a microwave oven. An ethanolic solution of the corresponding acetophenone was then added to sodium sulfinate and the reaction mixture was irradiated for 10 min to produce sulfones in good yields (1-13) (Scheme 2).

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Reference:
Article; Paloque, Lucie; Bouhlel, Ahlem; Curti, Christophe; Dumtre, Aurelien; Verhaeghe, Pierre; Azas, Nadine; Vanelle, Patrice; European Journal of Medicinal Chemistry; vol. 46; 7; (2011); p. 2984 – 2991;,
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. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 1,4-Diiodobutane

Stage 1 (0244) An oven-dried 3 L 4-neck flask fitted with an internal thermometer, N2 bubbler, overhead stirrer and oven-dried mL pressure-equalising dropping funnel was charged with 1,4-dibromo-2,5-diethylbenzene (70 g, 240 mmol) and dry THF (700 mL). The solution was cooled with stirring to <-70 C. to produce a white slurry. s-Butyllithium (335 mL, 1.4 M, 465 mmol) was charged to the dropping funnel and added dropwise over the space of 1.5 h ensuring the reaction temperature did not exceed -70 C. The slurry was stirred for 3 h after which GCMS confirmed the lithiation was complete. The dropping funnel was charged with a solution of 1,4-diiodobutane (13.8 mL, 105 mmol) in dry THF (140 mL) which was then added dropwise over 0.75 h. The resulting slurry was allowed to warm to room temperature and stirred for 12 h. The reaction was quenched by addition of water. The mixture was transferred to a separating funnel and the layers were separated. The aqueous layer was extracted with diethyl ether and the combined organics were washed with water, dried with MgSO4, filtered and concentrated to yield an orange oil. The product was triturated with 500 mL methanol for 0.5 h and filtered as a white solid before being recrystallised from toluene/IPA to yield a white powder that was dried in the oven (24.21 g, 48%). GCMS indicated a purity of 96% and the material was taken to the next stage without further purification The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings. Reference:
Patent; Cambridge Display Technology Limited; Sumitomo Chemical Company Limited; Kamtekar, Kiran; Steudel, Annette; (30 pag.)US9812644; (2017); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 21740-00-1, 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 21740-00-1 as follows.

2-(2-r(T2i?.5i?V5-([(‘5-Fluoropyridin-2-v?oxylmethvU-2-methylpiperidin-l-yl)carbonyll-4- methylphenvUpyrimidine (E-5)The solution of D-9 (1 kg, 4.46 mol) was charged in a visually clean and dry 50 L flask equipped with a thermocouple and mechanical stirrer and was solvent switched to DCM (11.00 L). DIPEA (2 L, 1 1.45 mol) is added and then EA (1.22 kg, 5.67 mol) was added to this stirring solution. This solution was cooled with an ice bath (12 C). To this stirring solution was added T3P (7.87 L, 13.38 mol) through an addition funnel keeping the reaction temperature <21 0C over Ih. Once addition was completed, the reaction became yellow and heterogenous. To facilitate stirring 2L of DCM were added. The reaction was heated to 44 0C (small exotherm at 42C, which causes the temperature to rise to 46.7 C and maintain that temperature for 30 min). The reaction was aged at this temperature overnight. After 17 h the reaction was not complete and T3P (1.1 L, 1.870 mol) was added to accelerate conversion. The next day (42 h) the reaction was deemed complete by HPLC and was cooled in an ice bath to 4 C. 20 L of water was added (slowly for the first 1.5 L then pretty fast.) keeping the reaction temperature under 17 0C. This mixture was stirred at room temperature for 30 minutes. Then the mixture was transferred into a 50 L extractor charged with 20 L of MTBE. The flask was rinsed with an additional 2 L of water and 4 L of MTBE. The layers were cut and the organics are washed with 20 L IN NaOH and then 10 L of IN NaOH. Finally, the organics were washed twice with 10 L of brine 15%. The organic fractions (quantitative HPLC assay at 1.65 kg) are then treated with ~50w% of Darco KB (75Og) for 1.75 h, filtered on Solka floe and rinsed with 10 mL/g of MTBE (1.559 kg, 94.5% recovery). To a visually clean and dry 50 L RBF equipped with a mechanical stirrer, a thermocouple, a reflux condenser and a nitrogen inlet was charged the crude material from above (E-5 solution and all solvents used were filtered using a 1 mum in-line filter). The reaction mixture was solvent switched to IPAc and the final volume was adjusted to 7.5 L (about 4 mL/g of IPAc). The reaction mixture was warmed to 75 0C (all soluble), cooled to room temperature slowly and seeded at 45 0C with 18 g OfE1S (front run material, obtained from rex in IP Ac/heptane) stirred overnight (16 hr) at room temperature then heptane was added (6 ml/g) over 60 min. The reaction mixture was aged for 1 hr before to be cooled to 5 0C and stirred for 30 min. The suspension was then transferred onto a filter pot and rinsed with IPAC/heptane (2 x 3mL/g of cold 15% IPAc) and heptane (5 mL/g). The residual beige solid was dried under a flow of nitrogen for 18 hr (the product was found to be dry with < 0.3 wt% of solvents). 1.2 kg of E-5 was isolated as a light beige solid (99.4 LCAP, > 99.5 % ee, > 99.5 % dr, Pd level of 8 ppm and KF of 0.1). Data for E^: HRMS m/z (M+H): 421.2067, found. 421.2035, required.

According to the analysis of related databases, 21740-00-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK & CO., INC.; WO2008/147518; (2008); 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. 628-77-3, name is 1,5-Diiodopentane, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1,5-Diiodopentane

Potassium carbonate (5.03 g, 36.44 mmol, 1.1 eq.) was added to a stirred solution of phenol (2) (14 g, 33.13 mmol, 1.0 eq.) and 1 ,5 diiodopentane (21.46 g, 9.86 mL, 66.26 mmol, 2.0 eq.) in DMF (250 mL). The solution was heated at 70C for 3.5h. The solution was poured into a mixture of ice/water (800 mL) and extracted with EtOAc (4 x 500 mL). The combined extracts were washed with H2O (2 x 250 mL), saturated brine (400 mL), dried (MgS04) and evaporated under reduced pressure to give a brown oil. Purification by flash column chromatography [n-heptane/EtOAc 40% to 80% in 10% increments] gave the product as a yellow foam (12.7 g, 85%). Analytical Data: LC/MS, RT 2.16 min; MS (ES+) m/z (relative intensity) 913 {[M + H]+, 100); 935 {[M + Na])+, 100).

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 628-77-3.

Reference:
Patent; MEDIMMUNE LIMITED; MASTERSON, Luke; VIJAYAKRISHNAN, Balakumar; CHRISTIE, Ronald, James; (118 pag.)WO2019/224340; (2019); A1;,
Iodide – Wikipedia,
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