Month: September 2021

Synthetic Route of 2142-70-3, These common heterocyclic compound, 2142-70-3, name is 1-(2-Iodophenyl)ethanone, 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.

[283] To a solution of 1-(2-iodophenyl)ethanone (4.0 g, 16.3 mmol) in a mixed solvent of chloroform (50 mL) and ethyl acetate (50 mL) was added cupric bromide (7.26 g, 32.5 mmol). The resulted mixture was stirred at reflux for 3h, then cooled down to roomtemperature, filtered, the filter cake was washed with ethyl acetate (50 mL), the filtrate was concentrated, the residue was purified by flash chromatography (petroleum ether: ethyl acetate= 50:1) to afford 2-bromo-1-(2-iodophenyl) ethanone (4.65 g, yield: 88%) as a light yellow oil.[284] ?H NIVIR (400 IVIFIz, CDC13-d): 7.98 (d, J = 8.0 Hz, 1H), 7.47 (d, J = 8.0 Hz, 2H), 7.19-7.21 (m, 1 H), 4.47 (s, 2H).

The synthetic route of 2142-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SHANGHAI DE NOVO PHARMATECH CO.,LTD.; LI, Qun; GAO, Daxin; (158 pag.)WO2016/131380; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 452-82-4,Some common heterocyclic compound, 452-82-4, name is 1-Fluoro-2-iodo-4-methylbenzene, molecular formula is C7H6FI, 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.

9A. 4-Bromomethyl-1-fluoro-2-iodo-benzene 4-Fluoro-3-iodotoluene (50 g, 210 mMol), N-bromosuccinimide (37.7 g, 212 mMol) and 2,2′-azobis-(2-methylpropionitrile) (348 mg, 2.12 mMol) were dissolved in carbon tetrachloride (300 mL) under an atmosphere of dry N2. The mixture was heated to reflux for 4 hours and then cooled to ambient temperature. The mixture was concentrated under vacuum and triturated with Et2 O. The filtrate was successively washed with water, aqueous saturated NaHCO3 and brine. The ether layer was dried over MgSO4, filtered and concentrated under vacuum to give a red oil. The oil was chromatographed on flash silica gel eluding with hexanes to give 33.8 g of the titled compound as a white solid.

The synthetic route of 452-82-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pfizer Inc.; US6150377; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 627-32-7, name is 3-Iodo-1-propanol, 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 627-32-7, Recommanded Product: 3-Iodo-1-propanol

K2CO3 (118mg, 0.86mmol), NaHCO3 (115mg, 1.36mmol) and, 3-iodo-1-propanol (0.06mL, 0.59mmol) were added to a solution of amine 19 (75mg, 0.39mmol) in acetone (4mL). The reaction mixture was heated to reflux. After 6h, the reaction was cooled to room temperature and the solvent was removed in vacuo. The reaction mixture was purified by chromatography (silica gel, gradient from CH2Cl2 to 95:5 CH2Cl2/MeOH) to afford compound 21 (66mg, 67%) as a brown solid; mp 85-87C; 1H NMR (400MHz, CDCl3) delta 3.77 (m, 2H), 3.13-3.00 (m, 2H), 2.66 (d, J=16.5Hz, 1H), 2.49 (dd, J=17.1, J=6.6Hz, 1H), 2.30-2.07 (m, 6H), 1.92 (m, 1H), 1.79 (m, 1H), 1.73-1.58 (m, 5H), 1.57-1.47 (m, 3H), 1.47-1.29 (m, 2H); 13C NMR (100MHz, CDCl3) delta 212.6, 64.5, 59.5, 48.5, 46.9, 44.3, 42.2, 39.0, 38.1, 35.8, 32.9, 27.8, 26.1, 25.6, 19.6; HRMS (ESI): m/z calcd for C15H26NO2 [M+H]+: 252.1958, found: 252.1962; FTIR (neat) numax: 3384, 2931, 2874, 1703, 1468, 1443, 1416, 1336, 1253, 1231, 1172, 1125, 1111, 1067, 733cm-1.

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:
Article; de Miguel, Irene; Velado, Marina; Herradon, Bernardo; Mann, Enrique; Tetrahedron; vol. 72; 31; (2016); p. 4617 – 4625;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route 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

Synthetic Route of 25309-64-2, These common heterocyclic compound, 25309-64-2, name is 1-Ethyl-4-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.

General procedure: To a stirred solution of aryl halides (1.0 mmol) and indoline/indoline carboxylic acid (1.0 equiv) in dry DMSO (2.0 mL) at rt was added nano CuO (5.0 mol %) followed by Cs2CO3 (2.0 equiv) and heated at 80 C for 8 h. The progress of the reaction was monitored by TLC. After the reaction was complete, the reaction mixture was cooled to room temperature and catalyst was filtered, the crude residue was extracted with ethyl acetate (3 × 10 mL). The combined organic layers were extracted with water, saturated brine solution, and dried over anhydrous Na2SO4. The organic layers were evaporated under reduced pressure and the resulting crude product was purified by column chromatography by using ethyl acetate/hexane (7:3) as eluent to give the corresponding N-substituted indoles in excellent yields. The identity and purity of the product were confirmed by 1H, 13C NMR, and mass spectra.

The synthetic route of 25309-64-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Reddy, K. Harsha Vardhan; Satish; Ramesh; Karnakar; Nageswar; Tetrahedron Letters; vol. 53; 24; (2012); p. 3061 – 3065;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 175278-30-5, 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. 175278-30-5, name is 4-Bromo-2-ethyl-1-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example R: Preparation of 4-bromo-2-ethylbenzaldehydeTo a solution of 4-bromo-2-ethyl-1-iodobenzene (75 g, 0.24 mol) in tetrahydrofuran (375 ml) at – 75 0C is added n-butyl lithium (1.6 M in hexanes, 196 ml, 0.31 mol) dropwise, maintaining the temperature of the reaction mixture below -70 °C. When the addition is complete the mixture is stirred at -75 0C for an additional 30 minutes and then lambda/,lambda/-dimethylformamide (70.7 g, 0.97 mol) is added dropwise. After the addition is complete the reaction is stirred at -75 °C for 2 hours, then allowed to warm to room temperature for 2 hours. The mixture is cooled in an ice bath and acidified with 0.5 N aqueous hydrochloric acid. The mixture is extracted with ethyl acetate (3 x 500 ml) and the organic fractions are combined, washed with brine, and dried over anhydrous sodium sulphate. The mixture is filtered and the filtrate is evaporated under reduced pressure. The residue is purified by column chromatography on silica gel to give 4-bromo-2- ethylbenzaldehyde (48 g) as an oil.

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-Bromo-2-ethyl-1-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SYNGENTA LIMITED; SYNGENTA PARTICIPATIONS AG; WO2009/74314; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 627-32-7,Some common heterocyclic compound, 627-32-7, name is 3-Iodo-1-propanol, molecular formula is C3H7IO, 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.

3. Preparation of 7-(2′-Trimethylsilanyl)ethyl-10-(3′-hydroxypropoxy) camptothecin (Compound 3) To a solution of 7-(2′-trimethylsilanyl)ethyl-10-hydroxy camptothecin (31 mg, 0.067 mmol) and potassium carbonate (15 mg, 0.11 mmol) in N,N-dimethylformamide (2 mL) was added 3-iodopropanol (0.1 ml) at -78 C. The resultant solution was stirred at room temperature for 16 hours. N,N-Dimethylformamide was removed by evaporation under reduced pressure. The residue was filtrated through silica gel with methanol/dichloromethane (10/90) and concentrated by rotary evaporation. Purification by radial preparative-layer chromatography (ethyl acetate/hexanes 50/50 to methanol/chloroform 2/98) provided 15 mg of 7-(2′-trimethylsilanyl)ethyl-10-(3′-hydroxypropoxy) camptothecin (Compound 3) as a yellow solid. 1H NMR (300 MHz, CDCl3) delta 8.02 (d, 1 H, J=9.3 Hz), 7.52 (s, 1 H), 7.34 (dd, 1 H, J1=9.3 Hz, J2=2.7 Hz), 7.14 (d, 1 H, J=2.7 Hz), 5.67 (d, 1 H, J=16.5 Hz), 5.22(d, 1 H, J=16.5 Hz), 5.09 (s, 2 H), 4.24-4.17 (m, 2 H), 3.90-3.85(m, 2 H), 3.00-2.88 (m, 2 H), 2.12-2.06 (m, 2 H), 1.90-1.76 (m, 2 H), 0.97(t, 3 H, J=7.3 Hz), 0.86-0.80 (m, 2H), 0.11 (s, 9 H). MS (m/z, M+1) 523.6

The synthetic route of 627-32-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BioNumerik Pharmaceuticals, Inc.; US2009/99166; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 111771-08-5, name is 2-Fluoro-6-iodobenzoic acid, 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 111771-08-5, Recommanded Product: 111771-08-5

To a 200 ml_ round- bottomed flask were added 2-fluoro-6-iodo-benzoic acid (7.5 g, 28.2 mmol), LiOH»H2O (1 .42 g, 33.8 mmol), and THF (100 ml_). The resulting mixture was warmed to 50 C and stirred for 2 h. Dimethyl sulfate (4.03 ml_, 42.3 mmol) was then added and the mixture was warmed to 65 C. After 2 h, the mixture was cooled to room temperature and NH4CI(aq) (50 ml_, 13 wt% solution) was added. The two resulting layers were thoroughly mixed and then separated. The organic layer was dried over MgSO4, filtered, and concentrated under reduced pressure to a light brown oil (7.79 g, 99% yield). 1H NMR (400 MHz, CDCIs): 7.68 – 7.60 (m, 1 H), 7.15 – 7.06 (m, 2H), 3.98 (s, 3H).

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-Fluoro-6-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.; WO2011/50200; (2011); 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. 2265-91-0, name is 1,3-Difluoro-5-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C6H3F2I

General procedure: To a solution of tetrabutylammonium bromide (1.100 g, 3.33 mmol), potassium acetate (0.586 g, 3.57 mmol), and palladium acetate (0.025 g, 0.11 mmol) in DMF (20 mL) were added substituted iodobenzene (2.21 mmol) and 4-acetyloxystyrene (2.44 mmol). The reaction mixture was recharged with Argon and stirred at 80C for 5 h in a sealed tube. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl and concentrated in vacuo. The residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 10:3) to afford the intermediate substituted (E)-4-styrylphenyl acetate. To a solution of triethylamine (2.0 mL) in MeOH (5 mL) was added substituted (E)-4-styrylphenyl acetate (1.36 mmol). The reaction mixture was stirred at reflux temperaturefor 3 h. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl and concentrated in vacuo. The residue was purified by column chromatography on silica gel (dichloromethane/methanol, 10:0.3) to afford pure product.

The synthetic route of 2265-91-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liang, Jian-Hua; Yang, Liang; Wu, Si; Liu, Si-Si; Cushman, Mark; Tian, Jing; Li, Nuo-Min; Yang, Qing-Hu; Zhang, He-Ao; Qiu, Yun-Jie; Xiang, Lin; Ma, Cong-Xuan; Li, Xue-Meng; Qing, Hong; European Journal of Medicinal Chemistry; vol. 136; (2017); p. 382 – 392;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 41252-96-4, name is 2-Chloro-1-iodo-4-nitrobenzene, 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 41252-96-4, Recommanded Product: 41252-96-4

EXAMPLE 34 (METHOD 8) 3-Chloro-4-trifluoromethyl-nitrobenzene A solution of 3-chloro-4-iodo-nitrobenzene (2.26 g), trimethyl(trifluoromethyl)silane (5.68 g), copper(I) iodide (2.28 g), and potassium fluoride (0.56 g) in N,N-dimethylformamide (8 mL) is heated in a sealed tube to 80 C. for 40 hours. The solution is then cooled, diluted with diethyl ether, filtered through diatomaceous earth, and the filtrate is washed successively with water, saturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure and the residue is chromatographed over silica gel (1% diethyl ether in hexanes followed by 10% ethyl acetate in hexanes is used as the eluant) to provided the desired product as a colorless oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-1-iodo-4-nitrobenzene, and friends who are interested can also refer to it.

Reference:
Patent; American Home Products Corporation; US6166028; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com