Month: May 2021

Electric Literature of 13101-40-1, 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 13101-40-1 as follows.

Nitrogen was passed into the three-necked flask equipped with mechanical stirring, thermometer and condenser,Add 100.0 mL of toluene, compound 5b-4 (20 mmol),Starting material 3-chloro-5-bromoiodobenzene (ie compound 5b-5, 21 mmol),Potassium carbonate (40 mmol), 20 mL ethanol, 20 mL water. Start stirring,The temperature was raised to 50 C, and tetrakistriphenylphosphine palladium (0.2 mmol) was quickly added.Continue heating to reflux state for 6h, pour into 100mL water with stirring,After standing, the liquid was separated, and the aqueous phase was extracted with 50 mL of toluene, and the organic phases were combined.Dry with 10g of anhydrous sodium sulfate, filter, and concentrate the filtrate (70 , -0.09MPa),Concentrate to distill off without solvent, add 50ml n-heptane,Filtration gave compound 5b-6 (17 mmol) in 85% yield.

According to the analysis of related databases, 13101-40-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanxi Laite Optoelectric Materials Co., Ltd.; Wang Jinping; Xue Zhen; Chen Zhiwei; (47 pag.)CN110981860; (2020); A;,
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. 141738-80-9, name is 3-Chloro-4-iodobenzotrifluoride, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 141738-80-9

General procedure: In a 4 mL screw-cap vial, 0.5 mmol of corresponding iodoarenecompound, 1.5 equiv of phenylacetylene or propargyl alcohol,0.005 equiv PdCl2(PPh3)2, and 0.8 mL of ionic liquid weremixed and stirred at 55 C for 3 h. After cooling, the mixturewas partitioned between 5 mL of water and 5 mL of pentane.After separation, the aqueous phase was extracted subsequentlywith 2 × 5 mL of pentane. The combined organic phase waswashed with brine, dried over MgSO4, filtered, and the solventwas evaporated under reduced pressure (ca. 10 mmHg). Theoily residue was purified by chromatography on silica gel(Merck Silicagel 60 (0.063-0.200 mm) for column chromatography(70-230 mesh ASTM)) eluted with n-pentane/EtOAc.The purity of the isolated products was >98%. The detailed experimentalprocedure as well as the characterization of isolatedcompounds are provided in Supporting Information File 1.

According to the analysis of related databases, 141738-80-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Orha, Laszlo; Tukacs, Jozsef M.; Kollar, Laszlo; Mika, Laszlo T.; Beilstein Journal of Organic Chemistry; vol. 15; (2019); p. 2907 – 2913;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 289039-25-4, A common heterocyclic compound, 289039-25-4, name is 3-Chloro-5-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

3-Chloro-5-iodobenzoic acid (D52, 4.72 g, 16.71 mmol) in dichloromethane (16.71 ml.) was added to a stirring solution of 1 ,1-dimethylethyl 2,2,2-trichloroethanimidoate (7.30 g, 33.4 mmol) in toluene (33.4 ml.) at room temperature under argon. Boron trifluoride etherate (0.334 ml_, 2.64 mmol) was then added to the mixture and left to stir for 18 hours. 1 ,1-Dimethylethyl 2,2,2-trichloroethanimidoate (7.30 g, 33.4 mmol) was added and the solution allowed to stir for another 6 hours. Solid sodium bicarbonate was added to the reaction mixture which was then filtered through silica and eluted with dichloromethane. The crude material (10.6 g) was then purified by flash chromatography (eluting with dichloromethane) to afford the title compound as a white solid.1H NMR delta (DMSOd6): 1.54 (9H, s), 7.85 (1 H, dd), 8.1 1-8.13 (2H, m)

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; GLAXO GROUP LIMITED; WO2009/819; (2008); 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 52914-23-5 as follows. Computed Properties of C8H9IO

EXAMPLE 10 Synthesis of Compound (1B) A mixture of 8.7 g (45 mmol) of 5H-dibenz[b,f]azepine, 12.4 g (50 mmol) of p-iodophenethyl alcohol, 2.8 g (50 mmol) of potassium hydroxide, 4. 8 g (75 mmol) of copper powder, and 20 ml of decalin was heated at an external temperature of 200 C. while stirring in a nitrogen stream for 40 hours. The reaction mixture was cooled nearly to room temperature, chloroform was added thereto, followed by filtration using Celite to remove any insoluble matter. The filtrate was concentrated. To remove decalin, n-hexane was added to the residue, followed by filtration. The filter cake was reprecipitated in methanol, and the resulting crude product was purified by silica gel column chromatography to give 4.2 g (30%) of 5-(4-(2-hydroxyethyl)phenyl)-5H-dibenz[b,f]azepine.

According to the analysis of related databases, 52914-23-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FUJI PHOTO FILM CO., LTD.; US2003/65171; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 13101-40-1,Some common heterocyclic compound, 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, molecular formula is C6H3BrClI, 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 a 250ml three-neck flask, nitrogen protection, was added 0.012mol 1- bromo-3-chloro-5-iodobenzene, 0.01 mol starting material A-3,150ml of toluene stirred and mixed, followed by addition of 5×10-5mol Pd2(dba)3,. 5 × 10-5mol tri-tert-butyl phosphate, 0.03 mol of sodium tert-butoxide and heated to 105 deg.] C, the reaction was refluxed for 24 hours, and sampling showed no residual amino compound, the reaction was complete; cool to room temperature, filtered, The filtrate was rotary evaporated until no fraction, through neutral silica gel column chromatography to give intermediate M-8, purity 99.8%, yield 89.6%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-3-chloro-5-iodobenzene, its application will become more common.

Reference:
Patent; Jiangsu March Optoelectric Technology Co., Ltd.; Zhao Sijie; Wang Fang; Xie Dandan; Wu Xiuqin; Zhang Zhaochao; (47 pag.)CN109836339; (2019); 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. 74128-84-0, name is 2-Bromo-1-iodo-3-methoxybenzene, A new synthetic method of this compound is introduced below., Safety of 2-Bromo-1-iodo-3-methoxybenzene

A mixture of 1-ethynyl-2-methylnaphthalene (3b) (500 mg, 3.6 mmol), 2-bromo-1-iodo-3-methoxybenzene (1.1 g, 3.6 mmol), Pd(PPh3)2Cl2 (105 mg, 0.15 mmol) and CuI (29 mg, 0.15 mmol), Et3N (5 mL) in THF (20 mL) was heated at 60 C for 2 h under nitrogen. The reaction mixture was cooled to room temperature and filtered through celite, and the precipitate was washed with ether. The organic layer was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography with ether and hexane (1 : 10) to give the title compound (661 mg, 63%) colorless crystals. mp 116-117 C; 1H-NMR (400MHz, CDCl3) delta8.56 (1H, d, J = 8.4 Hz), 7.82 (1H, d, J = 8.0 Hz), 7.76 (1H, d, J = 8.4 Hz), 7.59 (1H, t, J = 7.2 Hz), 7.47 (1H, t, J = 7.2 Hz), 7.38 (1H, d, J = 8.0 Hz), 7.34 (1H, d, J = 7.2 Hz), 7.30 (1H, t, J = 8.0 Hz), 6.90 (1H, d, J = 7.2 Hz), 4.08 (3H, s), 3.94 (3H, s); 13C-NMR (100MHz, CDCl3) delta156.6, 140.1, 133.8, 131.7, 128.7, 128.20, 128.18, 128.1, 127.6, 127.1, 126.2, 125.72, 125.67 119.2, 114.9, 111.7, 97.4, 91.4, 56.6, 21.8; IR (CHCl3)2936, 2837, 2203 cm-1; MS (EI) m/z (%, fragment) = 350 (100, M+), 307 (3.3, M+, -CH3O), 270 (7.2, M+,-Br); HRMS calcd for C20H15BrO: 350.0306. found 350.0314. Anal. Calcd for C20H15BrO: C, 68.39; H, 4.30. Found: C, 68.55; H, 4.03.

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; Kadoya, Nobuaki; Murai, Masato; Ishiguro, Masako; Uenishi, Jun’Ichi; Uemura, Motokazu; Tetrahedron Letters; vol. 54; 6; (2013); p. 512 – 514;,
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. 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H3BrClI

Weigh 1-bromo-3-chloro-5-iodobenzene and raw material A, dissolve it with toluene, and add Pd2(dba)3, tri-tert-butylphosphine and sodium t-butoxide; The mixed solution of the above reactants is reacted at a reaction temperature of 95 to 110 C under an inert atmosphere for 10 to 24 hours. Cooling and filtering the reaction solution, and the filtrate is steamed and passed through a silica gel column to obtain an intermediate M; The molar ratio of the starting material A to 1-bromo-3-chloro-5-iodobenzene is 1: (1.0-1.5), and the molar ratio of the Pd2(dba)3 to the raw material A is (0.005-0.01): 1 ,The molar ratio of the tri-tert-butylphosphine to the starting material A is (0.005-0.01): 1,The molar ratio of the sodium tert-butoxide to the raw material A is (1-3): 1, The toluene is used in an amount of from 100 to 150 ml of toluene per 0.01 mol of 1-bromo-3-chloro-5-iodobenzene

According to the analysis of related databases, 13101-40-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jiangsu March Optoelectric Technology Co., Ltd.; Zhao Sijie; Wang Fang; Xie Dandan; Wu Xiuqin; Zhang Zhaochao; (45 pag.)CN109912431; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 1012882-90-4, 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. 1012882-90-4, name is Ethyl 5-chloro-2-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

A degassed mixture of ethyl 5-chloro-2-iodobenzoate (0.621 g, 2.00 mmol), Pd(PPh3)4 (0.116 mg, 0.1 mmol), quinolin-6-ylboronic acid (0.381 g, 2.2 mmol), K2C03 (0.553 g, 4.0 mmol), dimethoxyethane (20 mL), and water (5 mL) was heated under reflux overnight. Solvents were removed under reduced pressure. The residue was diluted with sat’d NH4CI (15 mL) and extracted with EtOAc (3 x 30 mL). The combined organic layers were dried (MgSC^), concentrated in vacuo and purified by chromatography to afford ethyl 5-chloro-2-(quinolin-6-yl)benzoate (0.244 g, 39% yield) as a colorless oil. MS (ESI) m/z: 312.0 (M+H+).

The chemical industry reduces the impact on the environment during synthesis Ethyl 5-chloro-2-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; DECIPHERA PHARMACEUTICALS, LLC; FLYNN, Daniel L.; PETILLO, Peter A.; KAUFMAN, Michael D.; WO2013/36232; (2013); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

132554-73-5, name is 2-Fluoro-1-iodo-4-(trifluoromethyl)benzene, 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. SDS of cas: 132554-73-5

To a mixture of the 2-fluoro-1-iodo-4-(trifluoromethyl)benzene(580 mg, 2.0 mmol), tetrakis(triphenylphosphine)palladium(231 mg, 0.2 mmol), and CuI (381 mg, 2.0 mmol) in triethylamine at0 C was added tert-butyldimethyl(2-propynyloxy)silane (341 mg,2.0 mmol). The reaction mixturewas heated to 60 C for 30 min andthen filtrated through a short pad of silica gel. The residue waswashed with dichloromethane and the filtrate concentrated. Thecrude product was then purified by silica gel column chromatography(eluent, petroleum ether) to afford 17 as a brown oil. 1H NMR(400 MHz, CDCl3) delta 7.54 (t, J 7.4 Hz, 1H), 7.35 (dd, J 11.3, 8.9 Hz,2H), 4.58 (s, 2H), 0.92 (d, J 9.8 Hz, 9H), 0.17 (s, 6H).

The synthetic route of 132554-73-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wei, Hanwen; Mao, Fei; Ni, Shuaishuai; Chen, Feifei; Li, Baoli; Qiu, Xiaoxia; Hu, Linghao; Wang, Manjiong; Zheng, Xinyu; Zhu, Jin; Lan, Lefu; Li, Jian; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 235 – 251;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 116632-14-5, 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 116632-14-5 as follows.

8-(3-aminonaphthalen-2-ylthio)-9H-purin-6-amine (S13-4).; A mixture of 8- mercaptoadenine (20.7 mg, 0.124 mmol), neocuproine hydrate (3.9 mg, 0.0185 mmol), Cul (3.5 mg, 0.0185 mmol), sodium tert-butoxide (23.7 mg, 0.24 mmol), S13-3 (100 mg, 0.37 . mmol) and DMF (2 mL) were heated at 115C for 20 h. The solvent was removed under reduced pressure and the residue was purified by preparatory TLC (CH2Cl2:MeOH-NH3 (7N), 10:1) to give 14 mg (37%) of S13-4 as a solid. 1H NMR (500 MHz, CDC^/MeOH-cU) delta 8.18 (s, 1H), 8.12 (s, 1H), 7.71 (d, J= 8.3 Hz, 1H), 7.62 (d, J= 8.1 Hz, 1H), 7.40-7.46 (m, 1H), 7.24-7.30 (m, 1H), 7.20 (s, 1H); MS (ESI) m/z 308.95 [M+H]+.

According to the analysis of related databases, 116632-14-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SLOAN-KETTERING INSTITUTE FOR CANCER RESEARCH; CHIOSIS, Gabriela; TALDONE, Tony; SUN, Weilin; WO2011/44394; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com