Month: July 2021

Application of 3819-88-3,Some common heterocyclic compound, 3819-88-3, name is 1-Fluoro-3-iodo-5-nitrobenzene, molecular formula is C6H3FINO2, 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.

To a solution of 1.0 eq IA in dry DMF (0.37 M) was added Zn(CN)2 (0.92 eq) and Pd(PPli3)4 (0.058 eq). The reaction mixture was purged with nitrogen and heated to 800C overnight. An additional 0.023 eq of Pd(PPh3)4 was then added and the reaction was heated for another 6 hrs. The reaction mixture was then cooled to RT, diluted with 15 volumes of EtOAc (based on IA) and the organic layer was washed 3 times with water and once with brine. The organic layer was dried over sodium sulfate, filtered and concentrated. Purification by chromatography over silica gel using 10% Et2O/hexane as the eluant provided IB as a solid (90%).

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

Reference:
Patent; CYTOKINETICS, INC.; WO2007/70626; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 75581-11-2, 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. 75581-11-2, name is 4-Iodo-1-methoxy-2-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[00359] In a reaction tube under nitrogen, a mixture of PdCl2(dppf)CH2Cl2 (21 mg; 0.026 mmol) and triethylamine (0.34 ml; 2.44 mmol) in dioxane (2.5 ml; dried over 4 A sieves) was sealed and stirred at 80 C. overnight (18 h). After cooling to room temperature, HB(pin) (0.19 ml; 1.31 mmol) was added followed by 1-iodo-4-methoxy-3-methylbenzene (215 mg; 0.867 mmol) in dioxane (2.5 ml; dried over 4 A sieves) and the reaction mixture was stirred at 80 C. GC analysis after 18 hours showed a single new peak at 11.4 minutes which was identified by GC/MS as the desired arylborate compound.

The synthetic route of 4-Iodo-1-methoxy-2-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Commonwealth Scientific and Industrial Research Organisation; US6680401; (2004); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 450412-28-9, 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. 450412-28-9, name is 1-Bromo-3-chloro-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Intermediate A1 (95.2 g, 0.29 mol),1-Bromo-3-chloro-2-iodobenzene (109.1 g, 0.34 mol),Copper Iododide (54.5 g, 0.29 mol) and K3PO4 (182.1 g, 0.86 mol) were placed in dimethylacetamide (950 mL) and the mixture was refluxed and stirred.After the reaction was completed, the reaction solution was cooled to room temperature and then copper was removed by filtration. The solution in which the product was dissolved was reduced in pressure to remove all of the solvent. Then, the solution was completely dissolved in CHCl 3 and washed with water. The solvent was then removed under reduced pressure, and the resulting product was purified by column chromatography to obtain 132.1 g of intermediate A2 (yield: 88% .

The synthetic route of 1-Bromo-3-chloro-2-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LG Chem, Ltd.; Lee Jeong-ha; Park Tae-yun; Lee Dong-hun; Kim Min-jun; (39 pag.)KR2018/40100; (2018); 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. 55406-53-6, name is 3-Iodoprop-2-yn-1-yl butylcarbamate, A new synthetic method of this compound is introduced below., Recommanded Product: 55406-53-6

EXAMPLESA solution is prepared in Dowanol TPM (tripropylene glycol methyl ether), containing 10% by weight of iodopropargyl butylcarbamate, 5% by weight of Octasoligen-Cobalt 8 (Borchers, Langenfeld, Germany) and 5% by weight of the stabilizer specified in Table 1. The compositions are stored at 40 C. The amount of IPBC was determined by means of HPLC at the beginning and after two weeks.

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; Uhr, Hermann; US2009/36555; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 1878-69-9,Some common heterocyclic compound, 1878-69-9, name is 2-(3-Iodophenyl)acetic 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.

To a 125 mL round-bottom flask in a 0 C ice bath was added 3-iodobenoic acid (5.0 g, 23 mmol), EDCI (5.0 g, 26 mmol), DCM (50 mL) and allowed to stir for 10 min. To the stirred solution was added DMAP (0.3 mg, 2.3 mmol) and methanol (1.1 mL) and the reaction allowed to stir overnight. Disappearance of SM was monitored by HPLC. Reaction mixture was diluted with DCM, washed with 1 N HCI, dried with magnesium sulfate, and concentrated in vacuo. Required column chromatography (10: 1 Hex/EtOAc) to isolate product (4.56 g, 87%); LC rt = 3.77 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(3-Iodophenyl)acetic acid, its application will become more common.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; WO2005/70407; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, molecular formula is C8H6BrIO, 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. Quality Control of 2-Bromo-1-(4-iodophenyl)ethanone

General procedure: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 31827-94-8, its application will become more common.

Reference:
Article; Secci, Daniela; Bizzarri, Bruna; Bolasco, Adriana; Carradori, Simone; D’Ascenzio, Melissa; Rivanera, Daniela; Mari, Emanuela; Polletta, Lucia; Zicari, Alessandra; European Journal of Medicinal Chemistry; vol. 53; (2012); p. 246 – 253;,
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. 364-12-5, name is 5-Bromo-2-iodobenzotrifluoride, A new synthetic method of this compound is introduced below., name: 5-Bromo-2-iodobenzotrifluoride

A vial containing 4-bromo-l-iodo-2-(trifluoromethyl)benzene was charged with potassium phosphate (0.130 g, 0.614 mmol), followed by a solution of N-(2,4- dimethoxybenzyl)-l-methyl-3-(4,4,5,5-tetramethyl- 1,3, 2-dioxaborolan-2-yl)-N-( 1 ,2,4- thiadiazol-5-yl)-lH-indole-6-sulfonamide (Intermediate H) (0.100 g, 0.175 mmol) and PdCl2(dppf)-CH2Cl2 (0.014 g, 0.018 mmol) in 1 mL of DMF. The vial was sealed and placed in a shaker block. The block was shaken for three hours at 85 C. The solution was filtered, washed with DMF and concentrated. The resulting solid was treated with a solution of TFA (0.270 mL, 3.51 mmol) in 1 mL of DCM. The vial was shaken at room temperature for two hours. The solution was concentrated and purified via reverse phase HPLC (8 min. gradient elution 15 to 75% ACN/H20, 0.1% TFA modifier) to afford 3-(4- bromo-2-(trifluoromethyl)phenyl)-l-methyl-N-(l,2,4-thiadiazol-5-yl)-lH-indole-6- sulfonamide as an off-white solid.

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; DINEEN, Thomas; MARX, Isaac, E.; NGUYEN, Hanh, Nho; WEISS, Matthew; AMGEN INC.; WO2013/25883; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 32024-15-0, 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. 32024-15-0 name is 3-Iodo-4,5-dimethoxybenzaldehyde, 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.

2-Acetylnaphthalene (511 mg, 3.0 mmol) was dissolved in MeOH (10 mL) and 3-iodo-4,5-dimethoxybenzaldehyde (876 mg, 3.0 mmol) was added. 5% NaOH (3.0 mL) was added and the reaction mixture was stirred at room temperature for 16 h. The formed precipitate was collected, washed with MeOH and dried in vacuum. Yield: 1.127 g (2.54 mmol, 85%);

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Iodo-4,5-dimethoxybenzaldehyde, and friends who are interested can also refer to it.

Reference:
Article; Schmitt, Florian; Draut, Heidrun; Biersack, Bernhard; Schobert, Rainer; Bioorganic and Medicinal Chemistry Letters; vol. 26; 21; (2016); p. 5168 – 5171;,
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. 825-98-9, name is 3-Fluoro-4-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H4FIO2

To a solution of 3-fluoro-4-iodobenzoic acid (step-lof Intennediate-27, 1.0 g, 3.75 mmol) inDCM (20.0 mL) was added oxalyl chloride (947 mg, 7.57 mmol) and stirred at ft for 3-4 h.Meanwhile, to a solution of 2-(dimethylamino)ethanol (501 mg, 5.63 mmol) in THF (20.0 mL)was added Et3N (759 mg, 7.51 mmol) and stirred for 5-10 mins followed by addition of aboveprepared acid chloride solution. The reaction mass was stirred at rt for 16 h before it wasquenched with water and extracted with DCM. The organic layer was concentrated to afford400 mg of title product. ?H NMR (300 MHz, DMSO-d6): 10.54 (br s, 1H), 8.08-8.03 (t, J =7.8 Hz, 1H), 7.95-7.91 (d, J = 9.3 Hz, 1H), 7.68-7.66 (m, 1H), 4.59 (t, 2H), 3.50 (br s, 2H),2.84 (s, 6H); MS [M+Hj: 338.

According to the analysis of related databases, 825-98-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; GHARAT, Laxmikant Atmaram; MUTHUKAMAN, Nagarajan; PISAL, Dnyandeo; KHAIRATKAR-JOSHI, Neelima; SHAH, Daisy Manish; KADAM, Sheetal R; (303 pag.)WO2016/55947; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 20691-72-9, A common heterocyclic compound, 20691-72-9, name is 4-Iodo-2-nitroaniline, molecular formula is C6H5IN2O2, 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.

Preparation of (2-nitro-phenyl)-carbamic acid tert.-butyl esters from 2-nitroanilines Method a: To a solution of diphosgene (4.1 mL, 34.1 mmol) in EtOAc (40 mL) at 0 C. was added a solution of the 4-iodo-2-nitroaniline (45.5 mmol) in EtOAc (200-500 mL), and the mixture was heated to reflux for 18 h. The solvent was removed in vacuum to leave a brown solid, which was triturated with hot hexane (200 mL). The solid material was filtered off and the filtrate was concentrated under reduced pressure to leave the pure 4-iodo-2-nitrophenylisocyanate as a yellow solid.

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; Hoffmann-la Roche Inc.; US6407094; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com