Tag: M.W=200-300

Related Products of 460-37-7,Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, 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 168A Ethyl 3-ethyl-2,4-dioxo-5-(trifluoromethyl)-1-(3,3,3-trifluoro9propyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carboxylate 1.39 g (13.1 mmol) of caesium carbonate were added to a solution of 2.0 g (5.95 mmol) of the compound from Ex. 165A in 40 ml of DMF, and the mixture was stirred at RT for 15 min. Then 2.66 g (11.9 mmol) of 3,3,3-trifluoro-1-iodopropane were added, and the mixture was heated at 60 C. After 1 h, a further 2.66 g (11.9 mmol) of 3,3,3-trifluoro-1-iodopropane were added. Stirring at 60 C. was continued for 16 h. After cooling to RT, about 160 ml of water were added and the mixture was extracted three times with about 80 ml of diethyl ether each time. The combined organic extracts were washed with saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and the filtrate was evaporated. The crude product was purified by MPLC on a Puriflash cartridge (100 g of silica gel, cyclohexane/ethyl acetate 7:1?1:1). The product fractions were combined and concentrated, and the residue was dried under high vacuum. 1.86 g (72% of theory) of the title compound were obtained. 1H-NMR (400 MHz, CDCl3, delta/ppm): 4.41 (q, 2H), 4.20 (t, 2H), 4.08 (q, 2H), 2.73-2.61 (m, 2H), 1.40 (t, 3H), 1.26 (t, 3H). LC/MS (Method 1, ESIpos): Rt=1.15 min, m/z=433 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1-Trifluoro-3-iodopropane, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
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170112-66-0, name is 3,4,5-Trifluoroiodobenzene, 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. COA of Formula: C6H2F3I

1 mmol of cp-2-19 was dissolved in 10 ml of anhydrous acetonitrile and 0.05 mmol of Pd (OAc) 2,0.1 mmol of P (O-Tolyl) 3 and 3 mmol of Et3N, followed by addition of 1.5 mmol of 3,4,5-trifluoroiodobenzene and Ar gas for 12 h.After filtration, the filtrate was evaporated to dryness and the dichloromethane was dissolved, washed with water, washed with saturated NaCl and treated with anhydrous MgSO4. The silica gel column (PE: EA 50: 1)To the compound

The synthetic route of 170112-66-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Peking University; Fu, Hongzheng; Chen, Peng; (29 pag.)CN106543032; (2017); A;,
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Synthetic Route of 58313-23-8,Some common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, molecular formula is C9H9IO2, 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: The synthesis of the intermediate 13 was carried out by 3-p-benzoic acid ethyl ester (2.76 g, 10 mmol) and Intermediate 5 (2.45 g, 15 mmol) by the above method, and purified by column chromatography ( petroleum ether: ethyl acetate = 20:3) Obtained white oil intermediate 13 (2.17 g, 70%)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl-3-iodobenzoate, its application will become more common.

Reference:
Patent; Sun Yat-sen University; Gu Qiong; Xu Jun; Fang Yuying; (20 pag.)CN109879856; (2019); A;,
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618-91-7, name is Methyl 3-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. Recommanded Product: Methyl 3-iodobenzoate

To Methyl 3-iodobenzoate (25.0 g, 95.41 mmol) in ethanol (120.0 ml) was added hydrazine hydrate (50.0 ml). The reaction mixture was reflux for 18 hours. Heating was stopped and then water (300.0 ml) was added. After cooling down to room temperature, white solid was appeared. The white product solid was collected by filtration. The product was washed with water and dried under vacuum. Final white pure product was obtained in 23.0 g (92.0%). 1H NMR (400 MHz, DMSO-de, delta): 9.85 (s, br, 1 H, NH), 8.14 (t, J = 1.6 Hz, 1 H), 7.85 (m, 1 H), 7.82 (m, 1 H), 7.25 (t, J = 8.0 Hz, 1 H), 4.50 (s, 2 H, NH2). 13C NMR (100 MHz, CDCl3) delta: 168.54, 155.38, 129.54, 126.72, 125.57, 34.90, 31.07.

The synthetic route of 618-91-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GEORGIA TECH RESEARCH CORPORATION; ZHANG, Yadong; ZUNIGA, Carlos; DESHAYES, Gaelle; LEROY, Julie; BARLOW, Stephen; MARDER, Seth, R.; KIM, Sung-Jin; KIPPELEN, Bernard; WO2010/149620; (2010); A1;,
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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 452-82-4 as follows. Formula: C7H6FI

A mixture of 4-fluoro-3-iodotoluene (5.0 g, 21.2 mmol) and NBS (4.2 g, 23.3 mmol) in 50 mL of CCl 4 was refluxed under N 2 with benzoyl peroxide (250 mg, 1.03 mmol) was heated for 3 hours. The reaction mixture was cooled to room temperature and filtered through celite, washed with benzene. The filtrate was evaporated and pumped to give the benzylbromide as a crude light brown oil. [0192] A mixture of benzylbromide in 50 mL of DMSO was heated with NaHCO 3 solid (3.55 g, 42.2 mmol) at 120¡ã C. for 90 min. The reaction mixture was then cooled to room temperature, quenched with water, extracted with Et 2O, and washed with water, brine. The organic layer was dried with Na 2SO 4, concentrated in vacuuo. MPLC purification provided the titled compound as a colorless oil which solidified over time (2.2 g, 41.5% over two steps).

According to the analysis of related databases, 452-82-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Xin, Zhili; Liu, Gang; Pei, Zhonghua; Szczepankiewicz, Bruce G.; Serby, Michael D.; Zhao, Hongyu; US2004/214870; (2004); A1;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 117832-17-4, name is 2-Iodo-4,5-dimethylaniline, molecular formula is C8H10IN, 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. category: iodides-buliding-blocks

Preparation 2.65,6-Dimethyl-1 /-/-indole-3-carboxylic acid.(VIII): X = CH; R4 = Me; R5 = Me.Step 1 : 3-[(2-lodo-4,5-dimethylphenyl)amino]benzyl acrylate (XVIII).60.8 g of lithium chloride is added to a solution of 15.5 g of [1 ,4]- benzoquinone in 350 ml of THF, and it is degassed with nitrogen. 3.2 g of palladium acetate and 23.7 g of benzyl acrylate are added and it is degassed with nitrogen for about 30 minutes. Then a solution of 35.1 g of 2-iodo-4,5- dimethylaniline (prepared according to J. Med. Chem 2001 , 44, 3856-3871 ) in 150 ml of THF is added and it is stirred overnight. It is filtered and the filtrate is evaporated. The solid residue thus obtained is triturated with ether. It is filtered, the filtrate is washed with a solution of NaOH 0.5N and then with water and with brine. It is evaporated and then the solid residue is purified by silica gel chromatography, eluting with a cyclohexane/EtOAc mixture (8/2; v/v). 57.6 g of the expected compound is obtained in the form of a white powder.1H NMR: DMSO-de (250 MHz): delta (ppm): 2.14 (3H, s); 2.19 (3H, s); 4.93 (1 H, d); 5.18 (2H, s); 7.23 (1 H, s); 7.30-7.45 (5H, m); 7.59 (1 H, s); 7.72 (1 H, dd); 10.05 (1 H, d).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 117832-17-4, its application will become more common.

Reference:
Patent; SANOFI; BADORC, Alain; BOLDRON, Christophe; DELESQUE, Nathalie; FOSSEY, Valerie; LASSALLE, Gilbert; YVON, Xavier; WO2012/146318; (2012); A1;,
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Adding a certain compound to certain chemical reactions, such as: 1094759-93-9, name is 4-Chloro-5-fluoro-2-iodoaniline, 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 1094759-93-9, Recommanded Product: 1094759-93-9

Step C: 2-Amino-5-chloro-4-fluoro-benzonitrile A solution of 4-chloro-5-fluoro-2-iodo-phenylamine (2.5 g, 9.21 mmol) and copper (I) cyanide (1.65 g, 18.4 mmol) in DMA (45 ml) was heated to 130 C. overnight. Most of the DMA was removed under reduced pressure and the remaining residue was diluted with EtOAc and dichloromethane. The slurry was filtered and the filter cake was washed with dichloromethane and EtOAc. The filtrate was concentrated and the remaining residue was purified by column chromatography (silica gel, heptane/EtOAc 98:2-85:15) to afford the title compound (1232 mg, 78%) as light red solid. MS (ESI): 169.2 (M-H)-.

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Reference:
Patent; Hoffmann-La Roche Inc.; Ceccarelli, Simona M.; Conte, Aurelia; Kuehne, Holger; Kuhn, Bernd; Neidhart, Werner; Obst Sander, Ulrike; Rudolph, Markus; US2013/116234; (2013); A1;,
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. 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of Methyl 4-amino-3-iodobenzoate

A combined suspension of methyl 4-amino-3-iodobenzoate (3.0 g, 10.83 mmol), copper (_) iodide (41 mg, 0.22 mmol), bis(triphenylphosphine)palladium(II) dichloride (152 mg, 0.22 mmol), and 1-ethynyl-3-methoxybenzene (1.69 mL, 12.99 mmol) were stirred in toluene and TEA (1/1, 90 mL) at ambient temperature for overnight. The reaction solvent was evaporated under reduced pressure, and the residue was purified by column chromatography with hexane/ethyl acetate (3/1, v/v) to obtain the compound 47 as a white solid (3.00 g, 98% yield): 1H NMR (400 MHz, CDCl3) _ 8.07 (d, J = 2.1 Hz, 1H), 7.78 (dd, J = 8.2, 2.0 Hz, 1H), 7.21 (t, J = 7.9 Hz, 1H), 7.08 (dt, J = 7.7, 1.2 Hz, 2H), 7.03- 7.02 (m, 2H), 6.87- 6.86 (m, 1H), 6.66 (d, J = 8.6 Hz, 1H), 4.90 (s, 2H), 3.82 (s, 3H), 3.74 (s, 3H); 13C NMR (100 MHz, CDCl3) _ 166.5, 159.2, 151.7, 134.3, 131.3, 129.4, 123.8, 123.7, 118.8, 116.2, 114.8, 113.2, 106.7, 94.9, 84.6, 55.1, 51.6.

According to the analysis of related databases, 19718-49-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM; DALBY, Kevin N.; EDUPUGANTI, Ramakrishna; TALIAFERRO, Juliana; LEE, Juhyeon; (0 pag.)WO2018/160967; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 766-85-8,Some common heterocyclic compound, 766-85-8, name is 3-iodoanisole, molecular formula is C7H7IO, 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.

i) l-Bromo-2-iodo-4-methoxy-benzene Bromine (2.8 mL, 54.49 mmol) was added dropwise over 5 minutes to a solution of 3- iodoanisole (10.01 g, 42.77 mmol) in glacial acetic acid (65 mL). The resulting orange solution was stirred at room temperature for 24 hours. The reaction mixture was diluted with water and extracted with hexane. The combined extracts were washed with aqueous sodium thiosulfate solution (5%) and brine, dried over magnesium sulfate and concentrated under reduced pressure to give 13.51 g (quantitative yield) of the title compound. 1H NMR (400 MHz, CDCl3) delta ppm 7.47 (d, 1 H) 7.39 (d, 1 H) 6.77 (dd, 1 H) 3.77 (s, 3 H).

The synthetic route of 766-85-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; BYLUND, Johan; EK, Maria, E; HOLENZ, Joerg; KERS, Annika; OeHBERG, Liselotte; WO2010/132016; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 108078-14-4, 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 108078-14-4 as follows.

General procedure: To a solution of p-tolylhydrazine hydrochloride (0.79 g, 5 mmol), 2-chlorobenzoic acid (0.78 g, 5 mmol), and HCTU (2.28 g, 5.5 mmol) in DMF (10.0 mL), Et3N (2.08 mL, 15 mmol) was added. The mixture was stirred at r.t. overnight. Then the mixture was washed with sat. aq NH4Cl, aq NaHCO3, and brine. The organic layer was dried (MgSO4) and the solvent was removed under reduced pressure. The residue was purified by column chromatography (petroleum ether/EtOAc,5:1) to give 1b (0.78 g, 60%) as a white solid; mp 161.3-162.4 C.

According to the analysis of related databases, 108078-14-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Wang, Wei-Juan; Chen, Jia-Hua; Chen, Zi-Cong; Zeng, Yu-Feng; Zhang, Xue-Jing; Yan, Ming; Chan, Albert S. C.; Synthesis; vol. 48; 20; (2016); p. 3551 – 3558;,
Iodide – Wikipedia,
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