Month: December 2020

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. 33348-34-4, name is 4-Amino-3-iodobenzonitrile, A new synthetic method of this compound is introduced below., Product Details of 33348-34-4

To a solution of 4-amino-3-iodobenzonitrile in THF (4 ml.) was added BH3.THF (1 M solution in THF 2.5 ml.) drop-wise. The reaction mixture was refluxed for 3 h and 2 N HCI (1.0 ml.) was added . The resulting mixture was refluxed for an additional 1 h and then concentrated in vacuo in order to afford the crude, which was re-crystallized in MeOH for characterization to give 150 mg (74 %) of yellow powder. 4-amino-3-iodobenzylammonium chloride. ^ NMR (250 MHz, DMF) d 8.90 (s, broad, 3H, +NH3), 7.88 (d, J = 2.0 Hz, 1H, CHar), 7.42 (dd, J = 8.3, 2.1 Hz, 1H, CHar), 6.93 (d, J = 8.3 Hz, 1H, CHar), 5.81 (s, 6H, HCI), 4.06 (q, J = 5.6 Hz, 2H, CH2). (0104) 13C NMR (63 MHz, DMF) d 151.64 (Car-+NH3), 149.11(Car), 140.44 (CHar), 131.17 (CHar), 124.75 (Car), 114.86 (CHar), 82.93(Car-I), 42.30 (CH2).

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; UNIVERSIDAD COMPLUTENSE DE MADRID; FUNDACION PARA LA INVESTIGACION BIOMEDICA DEL HOSPITAL INFANTIL UNIVERSITARIO NINO JESUS; FUNDACION PARA LA INVESTIGACION BIOMEDICA DEL HOSPITAL UNIVERSITARIO LA PRINCESA; VALLET REGI, Maria; BAEZA GARCIA, Alejandro; VILLAVERDE CANTIZANO, Gonzalo; CASTILLO ROMERO, Rafael; RAMIREZ ORELLANA, Manuel; MELEN FRAJLICH, Gustavo; GONZALEZ MURILLO, Africa; ALFRANCA GONZALEZ, Arantzazu; (49 pag.)WO2019/185586; (2019); 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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 181765-86-6

In a 500-mL round-bottom flask reactor, methyl 5-bromo-2-iodobenzoate (25.0 g, 73 mmol), 4-dibenzofuran boronic acid (18.7 g, 88 mmol), tetrakis (triphenylphosphine)palladium (1.7 g, 0.15 mmol), and potassium carbonate (20.2 g, 146.7 mmol) stirred together with toluene (125 mL), tetrahydrofuran (125 mL), and water (50 mL) for 10 hrs at 80 C. After completion of the reaction, the reaction mixture was cooled to room temperature and extracted with ethyl acetate. The organic layer thus formed was separated, concentrated in a vacuum, and purified by column chromatography to afford . (75.0 g, 60.1%).

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC CO., LTD.; Pyo, Sung-Wan; Shim, So Young; Lee, Yun-Ah; Yu, Se Jin; (119 pag.)US2017/141321; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 77317-55-6, 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. 77317-55-6, name is Methyl 2-amino-5-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under an argon atmosphere 200 mg (0.72 mmol) 2-amino-5-iodo-benzoic acid methyl ester is dissolved in 4.0 ml toluene, 156 mg (0.94 mmol) 2-ethoxy-phenylboronic acid, a solution of 475 mg (2.17 mmol) tripotassium phosphate in 0.5 ml water, 53 mg (0.06 mmol) Pd2(dba)3, and 28 mg (0.10 mmol) N-phenyl-2-di-tert.-butylphosphinopyrrole are added. The reaction mixture is heated to 100 C. and stirred over night. After cooling to room temperature the reaction mixture is filterd over celite and the filtrate is evaporated under reduced pressure. The residue is purified by preparative HPLC (eluent A: water+0.13% TFA, eluent B: acetonitrile). The product is dissolved in dichloromethane and extracted with a saturated aqueous solution of Na2CO3. The organic layer is dried and evaporated under reduced pressure. yield: 40 mgRT (Microsorb 1s)=1.72 minESI-MS (M-FH)+=272

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-amino-5-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2010/249158; (2010); 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 61272-76-2 as follows. name: 4-Fluoro-2-iodoaniline

General procedure: A 25 mL Wattecs reaction tube was charged with 2-haloaniline 1 (0.6 mmol), potassium O-ethyl dithiocarbonate 2 (1.8 mmol),CuCl (0.06 mmol), and DMF (2 mL). The reaction vessel was flushed with argon three times and sealed. Then the mixture was stirred electromagnetically in an oil bath at 110¡ãC for 6 h.The reaction process was monitored by TLC on silica gel. After the reaction was completed, the reaction mixture was cooled to room temperature, and then HCl (3 mL, 3 mol/L) was added and stirred for another 30 min. The reaction mixture solution was extracted by ethyl acetate (3 ¡Á 20 mL). Subsequently, the combined organic solutions were dried by anhydrous sodium sulfate and the target product was purified by chromatography on a silica gel column (eluent: petroleum ether/ethyl acetate) togive the corresponding pure product 3. Complete characterization characterizationof the products (all known) is found in the Supplemental Materials (Figures S1?S13).

According to the analysis of related databases, 61272-76-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Lei; Zhu, Ning; Gao, Min; Zhao, Xiaole; Han, Limin; Hong, Hailong; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 191; 5; (2016); p. 699 – 701;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 83863-33-6, These common heterocyclic compound, 83863-33-6, name is 5-Iodo-2-methylaniline, 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.

9.97 g of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide (30.3 mmol) and 5.03 g of potassium iodide (30.3 mmol) in 75 ml. of cyclohexanol were stirred for 1 h at 800C. After addition of 7.7 g of sodium carbonate (72.7 mmol) and 5.65 g of 5-iodo-2-methyl- aniline (24.2 mmol), stirring continued for deltah at 1600C. At room temperature, the mixture was filtered, washed with dichloromethane, and the filtrate evaporated to dryness. The residue was dissolved in dichloromethane, filtered, and the solvent evaporated. The remaining residue was trituated with n-heptane and the crystalline product filtered off, washed several times with n-heptane and dried in vacuo to yield 10.7 g of product

The synthetic route of 83863-33-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBOTT GMBH &; CO. KG; ABBOTT LABORATORIES; HAUPT, Andreas; POHLKI, Frauke; DRESCHER, Karla; WICKE, Karsten; UNGER, Liliane; RELO, Ana-Lucia; BESPALOV, Anton; VOGG, Barbara; BACKFISCH, Gisela; DELZER, Juergen; ZHANG, Min; LAO, Yanbin; WO2010/125134; (2010); 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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C6H5ClIN

A solution of 3-CHLORO-4-IODO-ANILINE (5. 6G), ISOAMYLNITRITE (8. 8ML) and ETHYLDISULPHIDE (13. 4ML) in acetonitrile (100ml) was heated at 60C for 24h. The solvent was removed under reduced pressure and the residue purified by chromatography on silica eluting with 1% ETHYLACETATE/ISOHEXANE. YIELD 4. 02G ‘H NMR CDC13 : 8 7. 70 (1H, D) ; 7. 36 (1H, d); 6. 87 (1H, dd); 2. 94 (2H, q) ; 1. 32 (3H, t)

The synthetic route of 135050-44-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2004/89885; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 3032-81-3, A common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, molecular formula is C6H3Cl2I, 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.

General procedure: A suspension of DL-5-methoxypyrrolidin-2-one (3a) or arylaminopyrrolidinones 3b,c (1 equiv), CuI (0.5 equiv), cesium carbonate (2 equiv), and corresponding aryl iodide (1 equiv) in dioxane was placed under a nitrogen atmosphere. The coupling ligand DMEDA (1 equiv) was added dropwise by using a syringe and the mixture was then stirred at 60 ¡ãC for various periods of time (14?88 h). At the end ofthe reaction, the insoluble salts deposited after cooling at r.t. were collected by filtration then washed with dichloromethane. The resulting filtrate was concentrated in vacuo and the residue was partitioned between water and dichloromethane. The organic layer was dried on MgSO4 and evaporated to dryness. The residue was finally purified by chromatography on silica gel column (EtOAc/n-heptane) to afford pure N-arylated compound 40?44.

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Baudelet, Davy; Daich, Adam; Rigo, Benoit; Lipka, Emmanuelle; Gautret, Philippe; Homerin, Germain; Claverie, Christelle; Rousseau, Jolanta; Abuhaie, Cristina-Maria; Ghinet, Alina; Synthesis; vol. 48; 14; (2016); p. 2226 – 2244;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 450412-28-9, name is 1-Bromo-3-chloro-2-iodobenzene, 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 450412-28-9, Recommanded Product: 1-Bromo-3-chloro-2-iodobenzene

Step 1: 1-bromo-3-chloro-2-cyclopropylbenzene The mixture of 1-bromo-3-chloro-2-iodobenzene (7 g, 22.1 mmol), cyclopropylboronic acid (3.8 g, 44.2 mmol), Pd (dppf) Cl 2 (1.6 g, 2.21 mmol) and K 2CO 3 (2 g, 7.3 mmol, 1.0 eq) in dioxane (100 mL) was heated at 70 C for 12 hours under N 2 protection. TLC showed the reaction was complete and a new spot formed. The mixture was cooled to room temperature and was diluted with EtOAc (150 mL) and H 2O (50 mL). The organic phase was separated and washed with water (150 mL), brine (150 mL), dried over Na 2SO 4, and concentrated. The residue was purified by column chromatography on silica gel (eluent: PE) to give 1-bromo-3-chloro-2-cyclopropylbenzene (3 g, crude), which was used directly in next step.

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; BEIGENE, LTD.; GUO, Yunhang; XUE, Hai; WANG, Zhiwei; SUN, Hanzi; (493 pag.)WO2019/210828; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 32024-15-0, 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. 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

13as) In analogy to Example 13ap), from 3-iodo-4,5-dimethoxy-benzaldehyde and hydroxylamine hydrochloride there is obtained the corresponding 3-iodo-4,5-dimethoxy-benzaldehyde oxime as a colourless solid. Yield: 99%.

The synthetic route of 3-Iodo-4,5-dimethoxybenzaldehyde has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; US5763450; (1998); 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. 626-01-7, name is 3-Iodoaniline, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C6H6IN

General procedure: In a 10-ml round-bottom flask equipped with a condenser, a mixture of the aromatic amine (2 mmol), ethyl acetoacetate (1 mmol), and [Pyridinium-SO3H]HSO4 (0.0,385 g, 15 mol %) was stirred at 100 C for 10 min. Afterwards, the aromatic aldehyde (2 mmol) was added, and the resulting mixture was kept under stirring for the specified time in Table 3, the progress of the reaction was followed by TLC. After completion of the reaction, the reaction mixture was cooled to room temperature, extracted by the warm EtOAc (10 ml) to separate the catalyst. EtOAc was removed and the crude product was recrystallized from aqueous ethanol (96 %) to afford the pure product, which required no further purification. The recovered catalyst was washed with EtOAc (2 x 10 ml), dried, and reused, without considerable catalytic activity decrease.

According to the analysis of related databases, 626-01-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Mohammadi, Sedigheh; Abbasi, Mohsen; Research on Chemical Intermediates; vol. 41; 11; (2015); p. 8877 – 8890;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com