Tag: M.W=200-300

Electric Literature of 401-81-0, The chemical industry reduces the impact on the environment during synthesis 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

General procedure for N-arylation of amines:The N-nucleophile (1.47 mmol), Cu2O (Sigma-Aldrich, 99.99% purity, 0.147 mmol), K3PO4 (2.94 mmol), the aryl halide (1.76 mmol), phase transfer catalyst (0.147 mmol) and water (0.75 mL) were added to a reaction vial and a screw cap was fitted to it. The reaction mixture was stirred under air in a closed system at 130 C for 24 h, then the heterogeneous mixture was cooled to RT and diluted with dichloromethane. The resulting solution was directly filtered through a pad of Celite. The combined organic extracts were dried with anhydrous Na2SO4 and the solvent was removed under reduced pressure. The crude product was purified by silica-gel column chromatography to afford the N-arylated product. The identity and purity of all products was confirmed by 1H and 13C NMR spectroscopic analysis.

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-Iodo-3-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Yong, Fui-Fong; Teo, Yong-Chua; Tay, Siew-Hoon; Tan, Bryan Yong-Hao; Lim, Kim-Huat; Tetrahedron Letters; vol. 52; 11; (2011); p. 1161 – 1164;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 612-55-5, name is 2-Iodonaphthalene, 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 612-55-5, Recommanded Product: 2-Iodonaphthalene

General procedure: A definite amount of palladium catalyst and base were placed in an oven dried 25 mL Schlenk tube, and the reaction vessel was evacuated and filled with nitrogen for three times. Aromatic halide(0.5 mmol), phenylboronic acid (0.75 mmol), and solvent (5.0 mL) were added with a syringe, and the resulting mixture was stirred at 100 C for a desired time. After cooled down to room temperature, the reaction mixture was filtered and washed with brine and diethyl ether. The combined organic layers were washed with a saturated solution of sodium hydrogen carbonate and then with brine,dried over Na2SO4. Solvent was removed under a reduced pressure,and the reaction products were purified by silica gel chromatography with a mixture of n-hexane and ethyl acetate

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-Iodonaphthalene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chen, Liyu; Gao, Zhiqiang; Li, Yingwei; Catalysis Today; vol. 245; (2015); p. 122 – 128;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 20691-72-9, 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. 20691-72-9 name is 4-Iodo-2-nitroaniline, 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.

4-iodo-2-nitroaniline (2.64 g, 10.0 mmol)Was dissolved in 80% ethanol (60 mL)Concentrated hydrochloric acid (2.5 mL) was added.Iron powder (2.23 g, 40.0 mmol) was added,And the mixture was heated under reflux for 6 hours under stirring.After returning to room temperature,The precipitate was filtered,The solvent was distilled off under reduced pressure.After extraction with ethyl acetate (100 mL × 2) and saturated aqueous sodium hydrogen carbonate solution,The organic layer was washed with saturated brine.After dehydration with anhydrous magnesium sulfate,The solvent was distilled off under reduced pressure,The residue was subjected to silica gel column chromatography using ethyl acetate / hexane (1/1 (volume ratio)) as an elution solvent,Compound 9 was obtained in a yield of 1.98 g (89.1%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Iodo-2-nitroaniline, and friends who are interested can also refer to it.

Reference:
Patent; Kyoto University; Nihon Medi-Physics Co.,Ltd.; Saji, Hideo; Ono, Masahiro; Inohara, Tadashi; Seki, Ikuya; (24 pag.)JP2016/79108; (2016); 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. 202982-67-0, name is 4-Chloro-3-fluoroiodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 202982-67-0

A few drops of l -chloro-2-fluoro-4-iodobenzene (31.1 g, 121 mmol) in 50 mL of diethyl ether was added to the mixture of magnesium turnings (3.29 g, 136 mmol) and diethyl ether (50 mL) under nitrogen. After the reaction was initiated, the rest of the l-chloro-2-fluoro-4-iodobenzene ether solution was added at room temperature, and the reaction mixture was stirred at the same temperature for 1 h. This grignard reagent solution was added slowly to a solution of tert-butyl 4-(l-cyano-2- methoxy-2-oxoethy lidene)piperi dine- 1-carboxy late (10 g, 35.7 mmol) and copper(I) iodide (1.631 g, 8.56 mmol) in THF (200 mL) at 0 C, and the reaction mixture was stirred at 0 C for 1 h. Saturated ammonium chloride solution (100ml) was added, and the mixture was diluted with 500ml of ethyl acetate. The organic layer was washed with the water and brine solution, dried with the sodium sulphate and concentrated. The crude product was purified via silica gel chromatography eluteing with 20% of ethyl acetate in pet ether to give tert-butyl 4-(4-chloro-3-fluorophenyl)-4-(l-cyano-2-methoxy-2- oxoethyl)piperi dine- 1-carboxy late (12 g, 77%).

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; BRISTOL-MYERS SQUIBB COMPANY; WU, Yong-Jin; GUERNON, Jason M.; (102 pag.)WO2018/81384; (2018); 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 20555-91-3 as follows. SDS of cas: 20555-91-3

Alternative Preparation of 2-(3,4-dichloro-phenylamino)-propionic Acid; A mixture of 3,4-dichloroiodobenzene (1.50 g, 5.50 mmol), L-alanine (734 mg, 8.25 mmol), copper(I) iodide, 2-hydroxybenzaldehyde phenylhydrazone (233 mg, 1.10 mmol), tri-potassium phosphate (3.50 g, 16.5 mmol), and N,N-dimethylformamide (8 mL) was stirred at 80 C. for 40 h, then after cooling diluted with water and acidified to pH 3 by addition of 37% aq. HCl solution. The mixture was extracted with EtOAc, the organic phase was washed with brine, dried (MgSO4), filtered, and evaporated. Chromatography (SiO2; EtOAc) afforded the title compound (1.08 g, 67%) as a 71:29 mixture of the (S) and (R) stereoisomers (accordingly, when D-alanine was used instead of L-alanine as starting material, the title compound was obtained as a 29:71 mixture of the (S) and (R) stereoisomers). Brown solid, MS: 232.1 (M-H)-.

According to the analysis of related databases, 20555-91-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Adam, Jean-Michel; Aebi, Johannes; Binggeli, Alfred; Green, Luke; Hartmann, Guido; Maerki, Hans P.; Mattei, Patrizio; Ricklin, Fabienne; Roche, Olivier; US2010/22518; (2010); 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. 2786-00-7, name is 5-Iodo-2-methoxybenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-Iodo-2-methoxybenzoic acid

5-iodo-2-methoxybenzoic acid (2.0 g, 7.2 mmol) was suspended in anhydrous dichloromethane (40 ml). To this suspension was added, with stirring under nitrogen, oxalyl chloride (0.754 ml, 8.62 mmol). N,N-dimethylformamide (0.035 ml) was then added dropwise to the reaction mixture, and the mixture stirred for 1 hour at room temperature. When the intermediate acid chloride was fully formed as demonstrated by LC/MS, isopropanol (20 ml) was slowly added, then after 15 minutes solid sodium bicarbonate (2 g) was slowly added. The reaction was diluted with 40 ml of 1:1 saturated sodium bicarbonate and water, and the aqueous phase extracted with dichloromethane (3*40 ml). The organic extracts were combined, dried over magnesium sulfate, and solvent removed under reduced pressure. The residue was purified by column chromatography (0 to 50% ethyl acetate in hexanes) to afford isopropyl 5-iodo-2-methoxybenzoate as an oil (1.6 g, 5.0 mmol). 69% yield. 321 (M+1).

According to the analysis of related databases, 2786-00-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Gilead Sciences, Inc.; US2012/4267; (2012); A1;,
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. 41252-96-4, name is 2-Chloro-1-iodo-4-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 41252-96-4

General procedure: A mixture of aryl halide (1.0 mmol), PdCl2 (0.05 mmol), PPh3 (0.10 mmol), CuI (0.1 mmol) and K2CO3 (2.0 mmol) was stirred in H2O (5 mL) at room temperature under an argon atmosphere. 2-Chloro-3-propargylaminoquinoxaline (2) (1.20 mmol) was added, and the mixture stirred at 70 C for 12 h. After completion of the reaction, the resulting solution was concentrated in vacuo, and the crude residue subjected to column chromatography (silica gel) using CHCl3-CH3OH (98:2) as an eluent to afford the pure product (Table 1).

The synthetic route of 41252-96-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bakherad, Mohammad; Keivanloo, Ali; Samangooei, Shahrzad; Tetrahedron Letters; vol. 53; 12; (2012); p. 1447 – 1449;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 103440-52-4, The chemical industry reduces the impact on the environment during synthesis 103440-52-4, name is Methyl 2-Iodo-5-methylbenzoate, I believe this compound will play a more active role in future production and life.

Methyl 5-methyl-2~(4 A5.54etramethyl- 1 ,3.2-dioxaborolan-2-yDbenzoate (B-2)A solution of B4 (5.9 kg, 21.37 mol) in iPAc was charged in a visually clean 100 L reactor equipped with a mechanical stirrer and thermocouple. The solution was solvent switched to 2-MeTHF (-35 L). Triethylamine (8.94 L5 64.1 mol) was added and the solution was degassed with N2- Pinacol borane (4.65 L, 32.1 mol) was added slowly (over 15 mins) to the stirring solution while maintaining the purge. The solution was further degassed for 10 min and tri-o-tolylphosphine (0.325 kg, 1.069 mol) was added followed by palladium (II) acetate (0.120 kg, 0.534 mol). This caused the reaction to turn black immediately with a slow exotherm from 11.5 0C to 30 0C. At this point a delayed exotherm was observed and the reaction temperature increased to 60 0C (over 45 min). The reaction temperature was increased to 77 0C and aged for another 45 min. At this point, HPLC analysis of a reaction aliquot revealed complete consumption of the starting material. The heat source was removed and an ice bath was placed under the flask to cool the reaction over 1.5 h. A 26 w% ammonium chloride solution was added very slowly to control gas evolution and exotherm (over 60 minutes) which caused a black precipitated to form. The supernatant was transferred to an extractor which already contained 40 L of water. The black slurry remaining was filtered on Solka-Floc and washed with MTBE (-20 L). The filtrate was loaded into the extractor. The layers were cut and assay of the organic layers revealed R-2 (4.45 kg, 16.11 mol, 75 % yield) in 81.6% purity and was used as is in the following step. lH NMR (500 MHz, CDC13, 293K, TMS); 7.75 (1 H, s), 7.40 (1 H, d, J = 7.49 Hz), 7.32 (1 H, d, J = 7.56 Hz)5 3.90 (3 H, s), 2.37 (3 H5 s), 1.41 (12 H5 s).

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, Methyl 2-Iodo-5-methylbenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK & CO., INC.; MERCK FROSST CANADA LTD.; WO2009/143033; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 108078-14-4, name is 2-Iodo-3-methylbenzoic acid, molecular formula is C8H7IO2, 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. Product Details of 108078-14-4

General procedure: A mixture of 2-iodobenzoic 1a (0.2 mmol), acetylacetone 2a (0.4 mmol), and Cs2CO3 (65.2 mg, 0.20 mmol) in CH3CN was stirred at 100 C. When the reaction was considered complete as determined by TLC analysis, the reaction was allowed to cool to room temperature and quenched by water, and the mixture was extracted with CH2Cl2. The combined organic extracts were washed with water and saturated brine. The organic layers were dried over Na2SO4, filtered. Solvents were evaporated under reduced pressure. The residue was purified by chromatography on silica gel to afford isocoumarins derivatives and isoquinolone derivatives.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108078-14-4, its application will become more common.

Reference:
Article; Liu, Lei; Hu, Jie; Wang, Xiang-Chuan; Zhong, Mei-Jin; Liu, Xue-Yuan; Yang, Shang-Dong; Liang, Yong-Min; Tetrahedron; vol. 68; 27-28; (2012); p. 5391 – 5395;,
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. 618-91-7, name is Methyl 3-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H7IO2

General procedure: To a mixture of Iodobenzene (1.0 mmol), styrene (1.2 mmol), NaOAc (1.5 mmol), Catalyst (0.007 mmol) and DMF (3mL) was added in round bottom flask. (No inert gas protection was needed.). The reaction was carried out at 120 C for 15 min. Upon completion of reaction as indicated by TLC, the reaction mixture was poured in crushed ice-water, extracted with ethyl acetate, dried over anhydrous Na2SO4, concentrated in vacuum to give crude product which was purified through column chromatography on silica gel (100-200) to afforded pure stilbenes in 90-98% yields.

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

Reference:
Article; Sharma, Sonam; Sarkar, Bibhas R.; Synthetic Communications; vol. 48; 8; (2018); p. 906 – 914;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com