Month: August 2021

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 723294-75-5 as follows. name: 3-Fluoro-5-iodobenzonitrile

A mixture of compound 1 (15mg, 0.085mmol), compound 2(25mg, 0.1mmol), Cs2CO3 (110mg, 0.34mmol), Pd(dba)2 (5mg, 0.0085mmol) and Xanphos (4mg, 0.0085mol) in DMF(1.0mL) were degassed under N2 and then heated to 100 C for lh. After cooled, the reaction mixture was filtered. The filtrate was washed with H2O, extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated to residue, which was purified by prep-TLC (EA/PE, 1/2, v/v) to give desired compound (13mg, 52% yield). LCMS: m/z, 296.1(M+H)+; 1HNMR (400MHz, CDCl3) delta 4.24~4.44(m, 4H), 6.32~6.35(m, 1H), 6.66 (s, 1H), 6.75(d, J=8.0Hz, 1H), 7.26~7.35(m, 1H), 7.50(d, J=7.6Hz, 1H), 7.64~7.73(m, 1H), 8.62(d, J=4.8Hz, 1H).

According to the analysis of related databases, 723294-75-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HUA MEDICINE (SHANGHAI) LTD.; CHEN, Li; BALDWIN, John J.; WU, Chengde; SHEN, Chunli; WO2014/124560; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 2043-53-0, name is 1-Iodo-1H,1H,2H,2H-perfluorodecane, molecular formula is C10H4F17I, 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 1-Iodo-1H,1H,2H,2H-perfluorodecane

(Example 1) A mixture of fluoroalkyl alcohols represented by C2F5(CF2CF2)nCH2CH2OH containing one with n=3 in an amount of 80 mol% and one with n=4 in an amount of 20 mol% was produced by a technique of alcoholification of a mixture of C2F5(CF2CF2)nCH2CH2I. 150g (310mmol) of this fluoroalkyl alcohol mixture, 22.3g (260mmol) of acrylic acid, 50g of toluene, 1.48g (7.78mmol) of p-toluenesulfonic acid and 0.05g of hydroquinone were charged into a 300mL glass reactor equipped with a stirrer and subjected to esterification reaction for 4 hours while distilling off water, to give the reaction mixture having a composition as shown in Table 1. This reaction mixture was charged into a still and subjected to distillation using a rectifier with a theoretical plate number of ten(10) and selecting a pressure inside the rectifier and a still temperature within a range of from 0.3 kPa to 15 kPa and a range of from 100C to 160C respectively depending on compounds to be distilled off, so that toluene, acrylic acid, unreacted alcohols, the fluorine-containing acrylic esters (n=3 and n=4) and substances of high boiling points were distilled off in this order. As a result, the mixture after distillation was given as the distillate which was obtained by cutting toluene, acrylic acid and the unreacted alcohols as an initial distillate and the substances of high boiling points as a final distillate, and thereby contained the fluorine-containing acrylic esters as a main component and had a composition as shown in Table 1. In Table 1, the compositions of the reaction mixture and the mixture after distillation were determined by gas chromatography. Table 1 Component Reaction mixture (excluding toluene) (mol%) Mixture after distillation (mol%)C8F17CH2CH2OH 2.19 NDC10F21CH2CH2OH 0.65 0.03C8F17CH2CH2OCOCH=CH2 74.93 79.81C10F21CH2CH2OCOCH=CH2 18.60 19.50 Other substances of high boiling points 3.63 ND As shown in Table 1, of the impurities contained in the reaction mixture, C8F17CH2CH2OH (n=3) and the substances of high boiling points were able to be removed by the distillation. As a result, the mixture of the fluorine-containing acrylic esters with a high purity was obtained. Specifically, only C10F21CH2CH2OH (n=4) was contained as the impurity in an amount of 0.03 mol%. In this example, an yield of the fluorine-containing acrylic esters was 85 mass%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2043-53-0, its application will become more common.

Reference:
Patent; DAIKIN INDUSTRIES, LTD.; EP1757577; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 19094-56-5,Some common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

2-Chloro-5-iodobenzoyl chloride (10.7 g, 35.5 mmol) was dissolved in methylene chloride (200 mL). The resulting mixture was cooled in an ice-water bath. To this mixture was added aluminum trichloride (10.4 g, 78.2 mmol) followed by the dropwise addition of a solution of anisole (4.2 g, 38.9 mmol) in methylene chloride (50 mL). After completion of the dropwise addition, the resulting mixture was warmed to room temperature and stirred for 3 hours. The reaction mixture was poured into ice water and quenched. 3 mol / L hydrochloric acid was added to the reaction mixture. The product mixture was separated into an aqueous phase and an organic phase. The aqueous phase was extracted with methylene chloride (150 mL x 2). The organic phases were combined, washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting crude product was purified by silica gel column chromatography (ethyl acetate: petroleum ether = 0-1: 100) to give 12.0 g of product in 91% yield.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-5-iodobenzoic acid, its application will become more common.

Reference:
Patent; SENJU Pharma Corporation Limited; Woo, Frank; (28 pag.)KR2015/81220; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 181765-86-6, 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 181765-86-6 as follows.

To a solution of 5-Bromo-2-iodo-benzoic acid methyl ester (24 g, 70.4 mmol) and methyl 2,2-difluoro-2- (fluorosulfonyl)acetate (13.5 mL, 105.6 mmol) inN-methyl-2-pyrrolidinone (80 mL) was added copper (I) bromide (1.21 g, 8.45 mmol). The reaction mixture was stirred at 100C for 5 hours. The reaction was filtered and partitioned between ethyl acetate and brine. The aqueous layer was extracted with ethyl acetate, and the organic layers were combined and dried over Na2SO4. After filtration, the solvent was removed in vacuo. The residue waspurified by silica gel column (0-4% Ethyl acetate in Petroleum ether) to give the 5-Bromo-2-trifluoromethyl-benzoic acid methyl ester (119.2 g, yield 96%) as yellow oil.

According to the analysis of related databases, 181765-86-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SANOFI; PASCAL, Cecile; PELLET, Alain; COURTEMANCHE, Gilles; CAMPBELL, Simon; (78 pag.)WO2019/8027; (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. 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 51560-21-5

Example 3.3; Synthesis of 2,5-diiodo- 1 ,4-hydroquinone; A solution of 2,5-diiodo- 1,4-dimethoxybenzene (3.0Og, 7.69 mmol) in 30 ml ofAnhydrous dichloromethane was cooled to -80C and BBr3 (19 ml, 16.93 mmol) was added drop wise. The mixture was allowed to rt and stirred for additional 12h, solid precipitate was formed, collected and then crystallized from ethanol-water. The trace of solvent was evaporated at reduced pressure(2.50 g, yield 90 %).

The synthetic route of 51560-21-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITA’ DEGLI STUDI DI BARI; CONSIGLIO NAZIONALE DELLE RICERCHE; UNIVERSITA’DEGLI STUDI DEL SALENTO; WO2008/96239; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 689291-89-2, name is 5-Bromo-2-iodobenzaldehyde, 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 689291-89-2, COA of Formula: C7H4BrIO

(Z)-l,2-bis(5-bromo-2-iodophenyl)ethene (18a). A solution of phosphonium salt 16a (3.84 g, 6.02 mmol) in THF (60 mL) was cooled to 0 C in a 250 mL Schlenk flask under nitrogen with stirring. Potassium ‘butoxide (815 mg, 7.12 mmol) was added portionwise and the resulting mixture was held at 0 C for 30 min. A solution of benzaldehyde 17a (1.7 g, 5.5 mmol) in THF (60 mL) was added dropwise at 0 C and the reaction was allowed to warm up to room temperature and left stirring for 24 h. The reaction mix was partitioned between 1 : 1 water: diethyl ether. The aqueous layer was removed and extracted with diethyl ether (3x) and the organics were dried with MgS04, filtered and the solvent removed under reduced pressure to provide an off white solid that was further purified by a short plug (Si02: 10% ethyl acetate in hexane) to yield 2.95 g (4.99 mmol, 91%) 82:18 Z:E of 18a as an off-white solid that was used without further purification. -NMR (400 MHz, CDC13) delta: 7.70 (d, 2H, J= 8.4 Hz), 7.05 (dd, 2H, J= 8.4, 2.4 Hz), 7.02 (d, 2H, J= 2.4 Hz), 6.58 (s, 2H); HRMS (FAB) m/z calculated for Ci4H8Br2l2 Pv ]; 587.7082, found 587.7067.

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, 5-Bromo-2-iodobenzaldehyde, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE JOHNS HOPKINS UNIVERSITY; TOVAR, John Dayton; CARUSO, Jr., Anthony; WO2011/127383; (2011); A2;,
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. 29289-13-2, name is 2-Iodo-4-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2-Iodo-4-methylaniline

In the reaction vessel, 1 mmol of 2-iodo-4-methylaniline, 1 mmol of benzaldehyde, and 2.4 mmol of potassium thiocyanate were added.Nickel/proline lithium complexes (the catalyst metal is nickel chloride, the ligand is lithium valine, the ratio of nickel chloride or nickel bromide to lithium vanadate is 1:1) 0.05 mmol,Sodium hydroxide 1 mmol, water 3 mL.After being placed under the microwave reactor,Set in a microwave reactor to 100 C was heated for 30 minutes at 150 W power, cooled to room temperature.The product was extracted with ethyl acetate and concentrated under reduced pressure. The product was purified by column chromatography to give a white solid with a yield of 90%.

According to the analysis of related databases, 29289-13-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Fujian Medical University; Ke Fang; Xu Yiwen; Xu Jianhua; Chen Xiaole; Lin Chen; Xu Shuqing; (8 pag.)CN107954945; (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. 6940-76-7, name is 1-Chloro-3-iodopropane, A new synthetic method of this compound is introduced below., COA of Formula: C3H6ClI

Example 2; [0060]Synthesis of (4SV3-((2S)-5-chloro-2-r2-(trifluormethv?phenyllpentanovU-4-phenyl-L3- oxazolin-2-one [Formula 36][0061]LHMDS (1 M solution in THF, 94.3 mL, 94.3 mmol) was added dropwise to a solution of the compound of Example 1 (27.5 g, 78.7 mmol) in THF (275 mL) at -15C. 1- Chloro-3-iodopropane (33 mL, 315 mmol) and DMPU (94.8 mL, 787 mmol) were added dropwise thereto at -15C. The mixture was stirred at -150C for 23 hours and at 00C for 15 hours, followed by addition of a 5% sodium chloride solution (275 mL) and MTBE (275 mL). The organic layer was washed with a 5% sodium chloride solution (275 mL) and concentrated under reduced pressure. The residue was extracted with a mixture of MTBE (140 mL) and heptane (140 mL) and with water. The organic layer was concentrated under reduced pressure and then azeotropically distilled with MTBE (55 mL) twice. Ethanol (83 mL) was added to the residue, followed by heating to 500C. After confirming the formation of a homogeneous solution, a small amount of seed crystals were added. After one hour at room temperature, filtration was performed. The crystals were washed with cold ethanol (15 mL) and dried under reduced pressure to obtain 17.5 g of the title compound (content: 92%, 94.6% de) in a yield of 51.3%.Ethanol (48 mL) was added to the resulting title compound (content: 92%, 16 g, 34.6 mmol), and the compound was completely dissolved by heating to 500C. The solution was gradually cooled to room temperature. The generated crystals were washed with cold ethanol (15 mL) and dried under reduced pressure to obtain 14.9 g of the title compound (content: 96.3%, 100% de) in a yield of 97.8%.1H-NMR (400 MHz, CDCl3): delta 1.64-1.72 (m, IH), 1.74-1.84 (m, IH), 1.98-2.09 (m, IH), 2.12- 2.23 (m, IH), 3.44-3.53 (m, 2H), 4.31 (dd, J = 3.2, 8.8 Hz, IH), 4.68 (dd, J = 8.8, 8.8 Hz, IH), 5.36 (dd, J = 3.2, 8.8 Hz, IH), 5.54 (dd, J = 4.8, 9.2 Hz, IH), 7.28-7.34 (m, 2H), 7.35-7.46 (m, 4H), 7.52-7.59 (m, 1 H), 7.60-7.68 (m, 2H).

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Eisai R&;D Management CO., LTD.; UEMURA, Toshiyuki; SASAKI, Takeo; HOSHINO, Yorihisa; ISOMURA, Minetaka; WO2010/98496; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 56096-89-0,Some common heterocyclic compound, 56096-89-0, name is 4-Fluoro-2-iodobenzoic acid, molecular formula is C7H4FIO2, 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 mixture of the appropriate benzoic acid (10.0 mmol) and oxalyl chloride (15 mmol) was stirred at 0C for 2 h. The oxalyl chloride was removed under reduced pressure.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Fluoro-2-iodobenzoic acid, its application will become more common.

Reference:
Article; Kong, Lu-Lu; Fan, Li-Yan; Chinese Chemical Letters; vol. 27; 6; (2016); p. 827 – 831;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 5460-32-2, 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. 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

Step E: A mixture of the intermediate prepared in Step D, (S)-tert-butyl 4-(4-ethynyl- 3-(methoxycarbonyl)phenyl)-2-methylpiperazine-l-carboxylate (716 mg, 2.0 mmol), 4-iodo-l,2- dimethoxybenzene (634 mg, 2.4 mmol), Cul (19.0 mg, 0.1 mmol), PdCl2(Ph3P)2(70 mg, 0.1 mmol), Et3N (0.56 mL, 202 mg, 4.0 mmol) and acetonitrile (2.0 mL) was irradiated in a microwave reactor, under argon at 120 °C for 20 minutes. The mixture was then cooled and chromatographed twice (silica gel, ethyl acetate in hexanes, 0-50percent, then ethyl acetate in dichloromethane, 7.5percent) to give the alkyne intermediate as a yellow oil (367 mg, 37percent). MS m/z 495.3 [M+H]+.

The chemical industry reduces the impact on the environment during synthesis 4-Iodo-1,2-dimethoxybenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; PTC THERAPEUTICS, INC.; CHEN, Guangming; DAKKA, Amal; KARP, Gary Mitchell; LI, Chunshi; NARASIMHAN, Jana; NARYSHKIN, Nikolai; WEETALL, Maria L.; WELCH, Ellen; ZHAO, Xin; WO2013/112788; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com