Month: July 2021

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. 167479-01-8, name is tert-Butyl (3-iodopropyl)carbamate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 167479-01-8

Part C A solution of 4-amino-2-ethoxymethyl-1-isopropylamino-1H-imidazo[4,5-c]quinolin-7-ol (0.11 g, 0.35 mmol) in 10 ML of N,N-dimethylformamide was placed under an atmosphere of nitrogen and was treated with cesium carbonate (0.23 g, 0.70 mmol).After 5 min of stirring the mixture was treated with tert-butyl 3-iodopropylcarbamate (0.12 g, 0.35 mmol) and heated to 65 C. After 60 h, the reaction mixture was cooled to ambient temperature and then poured into 100 ML of ice water which resulted in a cloudy suspension.The mixture was extracted with CHCl3 (5*25 ML).The combined organic extracts were then washed with brine (50 ML), dried over Na2SO4, filtered and concentrated under reduced pressure to yield a tan oil.Chromatography (95:5 CHCl3:(80:18:2 CHCl3:MeOH:NH4OH) gradient to 1:1 gave 0.040 g of [3-(4-amino-2-ethoxymethyl-1-isopropylamino-1H-imidazo[4,5-c]quinolin-7-yloxy)propyl] tert-butyl carbamate as a light tan solid. LC/MS (APCI) m/z 473 (M+H)+.

The synthetic route of 167479-01-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; 3M Innovative Properties Company; US2004/176367; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 40400-15-5,Some common heterocyclic compound, 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, molecular formula is C8H6IN, 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 flask was equipped with a magnetic stir bar and charged with 1Hpyrrole-2-carbaldehyde (2a; 19.0 mg, 0.2 mmol, 1.0 equiv), 2-bromophenylacetonitrile(1a; 39.2 mg, 0.2 mmol, 1.0 equiv), and K3PO4(63.6 mg, 0.3 mmol, 1.5 equiv). The flask was evacuated and filledwith N2, and then anhydrous DMSO (2.0 mL) was introduced via a syringe.The flask was heated in a 130 C oil bath for 24 h, at which timeTLC analysis [petroleum ether (bp 60-90 C)-EtOAc, 10:1] indicatedcomplete consumption of 2a and 1a. The reaction mixture was cooledto r.t. and added to a sat. solution of NaCl (20 mL) and extracted withEtOAc (3 × 10 mL). The combined organic layers were dried (Na2SO4)and filtered. The filtrate was concentrated, and the residue was purified by column chromatography on SiO2 [petroleum ether (bp 60-90C)-EtOAc, 10:1 to 30:1] to give 3am; Yield: 27.9 mg (67%); tan solid; mp 191.3-192.0 C.

The synthetic route of 40400-15-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Jiang, Zeng-Qiang; Miao, Da-Zhuang; Tong, Yao; Pan, Qiang; Li, Xiao-Tong; Hu, Ren-He; Han, Shi-Qing; Synthesis; vol. 47; 13; (2015); p. 1913 – 1921;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

82998-57-0, name is 3-Iodo-4-methylbenzoic acid, 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. Recommanded Product: 82998-57-0

Oxalyl chloride (1.739 g, 1.20 ml, 13.7 mmol) was added dropwise to a solution of 3-iodo-4-methyl benzoic acid (0.717 mg, 2.74 mmol) and dichloromethane (9 ml). N,N-dimethylformamide (1 drop) was added and the colorless solution stirred at room temperature for 1 h. The solution was concentrated to afford 3-iodo-4-methyl benzoyl chloride as a light yellow solid which was used without purification. 2-(4-amino-2-(trifluoromethyl)benzyl)isoindoline-1,3-dione (Ic) (0.922 g, 2.88 mmol) was added to a solution of 3-iodo-4-methyl benzoyl chloride (0.767 g, 2.74 mmol) in dichloromethane (5 ml) and the mixture stirred at room temperature for 30 min. Triethylamine (0.360 g, 0.50 ml, 3.56 mmol) was added and the solution stirred at room temperature for 1 h. The reaction mixture was partitioned between dichloromethane and saturated aqueous sodium bicarbonate solution. The aqueous phase was separated and extracted with dichloromethane. The combined organic phases were washed with water, brine, dried over anhydrous sodium sulfate, filtered and concentrated to afford a solid (N-(4-((1,3-dioxoisoindolin-2-yl)methyl)-3-(trifluoromethyl)phenyl)-3-iodo-4-methylbenzamide (Id)).

The synthetic route of 82998-57-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Apicore, LLC; Kovi, Ravishanker; Kannapan, Jayaraman; Thakor, Sanjay F.; Patel, Rajesh A; US2014/343282; (2014); 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 13421-13-1 as follows. Formula: C7H4ClIO2

3.35 g (153.18 mmol) of methyl 4,5-dimethyl-1H-pyrrole-3-carboxylate prepared in accordance with the literature (Synthetic uses of tosylmethyl isocyanide (TosMIC) Organic Reactions (Hoboken, N.J., United States) (2001), 57, No 418) and 4.63 g (16.4 mmol) of 4-chloro-2-iodo-benzoic acid are dissolved in 50 mL of acetonitrile. There are added thereto copper powder (45 (280 mg, 4.37 mmol) as well as caesium carbonate (14.25 g, 43.74 mmol). The reaction mixture is heated at reflux for 12 hours. The progress of the reaction is monitored by liquid chromatography (LC). The suspension is allowed to return to ambient temperature and is then filtered, washed with acetonitrile and evaporated to dryness. The residue is taken up in ethyl acetate. The solution is then washed with 1M hydrochloric acid and then with a saturated sodium chloride solution, it is dried over maganesium sulphate, filtered and then evaporated to dryness. The compound so obtained is purified over a silica gel column using dichloromethane and ethanol as solvents. (0126) Mass spectroscopy (ESI+): (0127) Empirical formula: C15H14ClNO2 (0128) monoisotopic mass=307.07 Da (0129) [M+H]+, measured: 308.12 (0130) (isotope ratios consistent with one chlorine atom)

According to the analysis of related databases, 13421-13-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Les Laboratoires Servier; Vernails (R&D) Limited; CASARA, Patrick; LE DIGUARHER, Thierry; HENLIN, Jean-Michel; STARCK, Jeroeme-Benoit; LE TIRAN, Arnaud; DE NANTEUIL, Guillaume; GENESTE, Olivier; DAVIDSON, James Edward Paul; MURRAY, James Brooke; CHEN, I-Jen; WALMSLEY, Claire; GRAHAM, Christopher John; RAY, Stuart; MADDOX, Daniel; BEDFORD, Simon; (72 pag.)US2016/152599; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 6940-76-7, 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 6940-76-7 as follows.

Anhydrous potassium carbonate (10.6 g, 6 eq) was added to a solution of 4-chloro-7-hydroxy-6-methoxyquinoline-3-carbonitrile (3 g,12.7 mmol) in DMF (30 mL)After stirring for half an hour,1-Chloro-3-iodopropane (13 g, 63.9 mmol) was added to the suspension and stirred at room temperature overnight.The reaction solution was diluted with water (500 mL)Dichloromethane extraction (250 mL X2),The organic phases were combined,Respectively, with water,Washed with a saturated saline solution,Dried over anhydrous sodium sulfate,filter,Concentrated under reduced pressure,Silica gel column chromatography gave 4-chloro-7- (3-chloro-propoxy) -6-methoxy-quinoline-3-carbonitrile (yellow solid, 3.1 g)Yield 77%.

According to the analysis of related databases, 6940-76-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Pharmaceuticals Holding Co., Ltd.; Wan, huixin; Shen, JingKang; Li, ChunLi; Han, yanan; Liu, Haiyan; Zhou, ZhaoLi; Li, Ping; Li, Yufeng; Chen, gang; Xu, Jia; (54 pag.)CN103848785; (2016); B;,
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. 153898-63-6, name is 2-Iodo-5-methoxyaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C7H8INO

General procedure: Bis(triphenylphosphine)palladium(ll) dichloride (32.1 mg, 45.8 muiotatauiotaomicronIota), copper(l) iodide (17.8 mg, 91 .5 muiotatauiotaomicronIota), 2-iodo-5-methoxyaniline (1 .2 g, 4.6 mmol), phenylacetylene (572.5 ml, 5.5 mmol), and diethylamine (10 ml) are refluxed until consumption of the starting materials monitored by TLC. The residue is chromatographed on silica gel (heptane/EE, 10/1 ) to afford 5- Methoxy-2-(phenylethynyl)aniline (818 mg, 3.7 mmol, 80 % of theory).1 H NMR (500 MHz, Chloroform-d) delta 7.54 (d, J = 6.7 Hz, 2H), 7.36 (q, J = 8.9 Hz, 7.7 Hz, 2H), 7.32 (q, J = 8.9 Hz, 8.5 Hz, 2H), 6.34 (dd, J = 8.5 Hz, 2.4 Hz, 1 H), 6.30 (d, J = 2.3 Hz, 1 H), 3.82 (s, 3H).

The synthetic route of 153898-63-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK PATENT GMBH; SCHRAUB, Martin; DOBELMANN-MARA, Lars; RIEDMUELLER, Stefan; (326 pag.)WO2018/149852; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 619-58-9, 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. 619-58-9, name is 4-Iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a test tube containing a magnetic bar was added aryl halide (1.0 mmol), CuCl2 (13.4 mg, 0.1 mmol), KOH (336 mg, 6.0 mmol), ethylene glycol(12 muL, 0.2 mmol), and DMSO/H2O (1.0 mL/0.5 mL). After flushing with argon, the mixture was stirred in a preheated oil bath at 120 C for 24 h. After cooled to ambient temperature, the reaction mixture was distributed in aqueous HCl (5 %) and ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous MgSO4, and concentrated under vacuum. The crude product was further purified by column chromatography (EtOAc/n-Hexane) to provide the phenols.

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, 4-Iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kim, Jihye; Battsengel, Oyunsaikhan; Liu, Yajun; Chae, Junghyun; Bulletin of the Korean Chemical Society; vol. 36; 12; (2015); p. 2833 – 2840;,
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. 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1,2-Dichloro-4-iodobenzene

A 3M solution of n-BuLi in hexane (24 mL) was added to anhydrous THF (60 mL) at -78 C., followed by the addition of a solution of compound X-A-49 (15 g) in anhydrous THF (10 mL) dropwise. The mixture was stirred for an hour, then compound X-B-49 was added dropwise. The resulting mixture was stirred at -78 C. for an additional hour then allowed to warm up gradually to room temperature. After stirring at room temperature for 3 hours, the reaction was quenched by adding a saturated aqueous NH4Cl solution dropwise. The separated organic layer was set aside. The aqueous was concentrated to remove most of the THF, then extracted with EtOAc (3×30 mL). The combined organic solution was dried over Na2SO4 and concentrated. The residue was purified by column chromatography eluting with petroleum ether/EtOAc (5:1) to give 9.5 g of compound X-C-49 in 54% yield.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 20555-91-3.

Reference:
Patent; Kalypsys, Inc.; US2005/234046; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 72373-82-1, These common heterocyclic compound, 72373-82-1, name is 1-Chloro-2-fluoro-3-iodobenzene, 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.

The compounds dibenzo[b,d]furan-2-ol (30g, 0.16mol), 1-chloro-2-fluoro-3-iodo-benzene (41.7g, 0.16mol) in 300ml DMF in a nitrogen atmosphere completely After dissolving, potassium carbonate (44.2 g, 0.32 mol) was added and the mixture was heated with stirring for 2 hours. The temperature was lowered to room temperature, and water was added to obtain a solid, which was purified by column chromatography (chloroform / hexane) to give Compound 1-A (60.5 g, yield: 90percent)

Statistics shows that 1-Chloro-2-fluoro-3-iodobenzene is playing an increasingly important role. we look forward to future research findings about 72373-82-1.

Reference:
Patent; LG Chem, Ltd.; Yoon Hong-sik; Hong Wan-pyo; Jeong Gyeong-seok; Kim Yeon-hwan; Yoon Hong-je; (49 pag.)KR2018/101265; (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. 89459-38-1, name is 2-Iodo-4-nitrobenzoic acid, A new synthetic method of this compound is introduced below., Application In Synthesis of 2-Iodo-4-nitrobenzoic acid

A flame-dried 3 L 3-necked flask was charged with Example 2.59.1 (51.9 g) and tetrahydrofuran (700 mL). The solution was cooled in an ice bath to 0.5 C., and borane-tetrahydrofuran complex (443 mL, 1M in THF) was added dropwise (gas evolution) over 50 minutes, reaching a final internal temperature of 1.3 C. The reaction mixture was stirred for 15 minutes, and the ice bath was removed. The reaction left to come to ambient temperature over 30 minutes. A heating mantle was installed, and the reaction was heated to an internal temperature of 65.5 C. for 3 hours, and then allowed to cool to room temperature while stirring overnight. The reaction mixture was cooled in an ice bath to 0 C. and quenched by dropwise addition of methanol (400 mL). After a brief incubation period, the temperature rose quickly to 2.5 C. with gas evolution. After the first 100 mL are added over 30 minutes, the addition was no longer exothermic, and the gas evolution ceased. The ice bath was removed, and the mixture was stirred at ambient temperature under nitrogen overnight. The mixture was concentrated to a solid, dissolved in dichloromethane/methanol and adsorbed on to silica gel (150 g). The residue was loaded on a plug of silica gel (3000 mL) and eluted with dichloromethane to give the title product.

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; AbbVie Inc.; Boghaert, Erwin R.; Bruncko, Milan; Doherty, George; Frey, Robin R.; Judd, Andrew S.; Phillips, Andrew C.; Song, Xiaohong; Souers, Andrew J.; Sullivan, Gerard M.; Tao, Zhi-Fu; US2019/153107; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com