Category: iodides-buliding-blocks

Related Products of 42860-04-8, 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. 42860-04-8 name is 4-Chloro-3-iodobenzoic acid, 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.

To a 1 L oven dried flask was added 225 mL of dry DMF, 9 niL of phenyl acetylene, 77 mL of DIEA, and 25 gm of 4- Chloro-3-iodo benzoic acid. The mixture was degassed by bubbling 10 psi N2 gas through a canula needle for 25 minutes. 2.02 gm of Pd2dba3 and 338 mg Of (O-ToIyI)3P were added and the resulting mixture stirred for 69 hours a 65 °C. The solution was cooled and 500 mL of saturated Na2S2O5 was added and shaken vigorously in a separatory funnel. The water portion was removed and a gelatinous film remained in the flask after pouring off of the organic layer. The organic layer was filtered through coarse filter paper into a 4 L Erlenmeyer flask to remove the remaining polymeric material and left to stand for 8 hours. No additional precipitation was observed. To the organic solution was added one liter of water followed by 500 mL of sodium metabisulfite. Precipitation of the product was observed and the solution cooled in an ice bath for an additional 2 hours. The precipitated solids were collected by filteration in a funnel and washed (3 x 500 mL) with ice water. The solids were dried over night under vacuum. 58.7 gm of large opaque crystals were recovered. The crystals were dissolved in 1 L of ethyl acetate (EtOAc) in a separatory funnel, washed (3 x brine, 3 x H2O), and dried with Na2SO4 for 1 hour. The solution was filtered and the solvent removed by rotary evaporatoration. Over night drying under vacuum resulted provided 18.57 g of product as plate like crystals (81.7percent yield). 1H NMR 400 MHz DMSO-d6: deltaH 11.52 (IH s), 7.88-7.20 (8H m); MS (ES”) m/z 256 (M-H); HPLC (214 nm), rt 4.94 min, 99.8percent.

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

Reference:
Patent; PROPHARMACON, INC.; WO2006/22955; (2006); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 103962-05-6, 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. 103962-05-6 name is 1-Iodo-4-(trifluoromethoxy)benzene, 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.

Example 14 Preparation of 3-(4-nitrophenethyl)-1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazole (C41) To a 100 mL flask were added 3-(4-nitrophenethyl)-1H-1,2,4-triazole (C38) (6.50 g, 29.8 mmol), potassium carbonate (8.23 g, 59.6 mmol), and copper(I) chloride (0.590 g, 5.96 mmol). The flask was sealed and placed under inert atmosphere, then N,N-dimethylformamide (99 mL), N1,N2-dimethylethane-1,2-diamine (1.28 mL, 11.9 mmol), and 1-iodo-4-(trifluoromethoxy)benzene (6.99 mL, 44.7 mmol) were added. The reaction mixture was stirred in a heating block warmed to 100 C., overnight. The reaction mixture was cooled to room temperature and poured into brine solution. The aqueous layer was extracted with ethyl acetate (3*100 mL). The combined organic layers were dried over magnesium sulfate, filtered, and concentrated. The resulting residue was purified by flash chromatography using 0-70% ethyl acetate/hexanes as eluent to provide the title compound (8.97 g, 79%): 1H NMR (400 MHz, DMSO-d6) delta 9.23 (s, 1H), 8.21-8.07 (m, 2H), 7.99-7.87 (m, 2H), 7.55 (dd, J=8.8, 1.8 Hz, 4H), 3.20 (dd, J=8.2, 6.2 Hz, 2H), 3.15-3.04 (m, 2H); 19F NMR (376 MHz, DMSO-d6) delta -57.06; 13C NMR (101 MHz, DMSO-d6) delta 163.73, 149.34, 146.85, 145.93, 142.91, 135.61, 129.69, 123.81, 123.30, 122.46, 121.26, 120.76, 118.71, 116.14, 32.94, 28.62; ESIMS m/z 379 ([M+H]+).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-4-(trifluoromethoxy)benzene, and friends who are interested can also refer to it.

Reference:
Patent; Dow AgroSciences LLC; Giampietro, Natalie C.; Crouse, Gary D.; Sparks, Thomas C.; Demeter, David A.; (145 pag.)US2017/64962; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, 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 31599-61-8, Application In Synthesis of 4-Iodo-1,2-dimethylbenzene

General procedure: To a stirred solution of aryl halide (1 mmol) in 2.5 mL heptane were added the alkene (1.5 mmol) and the internal standard (unde-cane, 0.3 mmol). An aqueous solution (2.5 mL) containing ligand 1or 2 (0.1 mmol), Na2PdCl4(0.005 mmol) and NaHCO3(1.5 mmol)was then added. The reaction mixture was heated at 100C for 18 h.The reaction mixture was cooled to room temperature. Once the organic phase has been recovered, the aqueous phase was washed twice with diethyl ether (2 × 2 mL). The combined organic phases were dried over anhydrous MgSO4 and heptane was removed under vacuum. The residue was purified by chromatography over a silica gel column. Elution with 10% ethyl acetate – heptane gave the expected bisaryl products as colorless oils.

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; Potier, Jonathan; Menuel, Stephane; Rousseau, Jolanta; Tumkevicius, Sigitas; Hapiot, Frederic; Monflier, Eric; Applied Catalysis A: General; vol. 479; (2014); p. 1 – 8;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic 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 61203-48-3, category: iodides-buliding-blocks

General procedure: To a stirred solution of 2-iodobenzoic acids a (10 mmol) in CH2Cl2, was added DCC (dicyclohexylcarbodiimide, 11 mmol), DMAP (Dimethylaminopyridine, 2 mmol) and alcohols b (10 mmol) in sequence. The resulting solution was stirred overnight at room temperature then filtered through a sand core funnel and washed with diethyl ether (2 x 40mL). The combined organic layers were washed with water, brine, dried over Na2SO4, and concentrated under reduced pressure. The crude material was purified by flash column chromatography to obtain the pure product c in moderate to good yields. To a soluton of 2-iodobenzoates c in Et3N (5 mL) was added PdCl2 (PPh3)2 (4 mol %) and CuI (2 mol %) and the reaction vial was flushed with Ar and the reaction mixture was stirred for 5 minutes. A solution of propargyl alcohols d (1.05 equiv) in Et3N (5 mL) were then added dropwise through a syringe for 5 minutes. The resulting solution was stirred at room temperature overnight. When the reaction was considered complete as determined by TLC analysis, the mixture was quenched by addition of saturated aqueous ammonium chloride (10 mL) and extracted with ethyl ether (3 x 40 mL). The combined organic layers were washed with water, brine, dried over Na2SO4, and concentrated under reduced pressure. The crude material was purified by flash column chromatography to give 1.

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-Iodo-4,5-dimethoxybenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhu, Hai-Tao; Tong, Xiao-Juan; Zhou, Ni-Ni; Yang, De-Suo; Fan, Ming-Jin; Tetrahedron Letters; vol. 57; 49; (2016); p. 5497 – 5500;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 27913-58-2, 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. 27913-58-2, name is 4-(4-Iodophenyl)butanoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step A: Preparation of methyl 4-(4-iodophenyl)-butyrate To a solution of 4-(p-iodophenyl)-butyric acid (45.0 g, 0.155 mol) in methanol (1.3 L), was added sulfuric acid (concentrated, 8.4 mL) dropwise and it was stirred at room temperature under nitrogen for 3 hours. The reaction mixture was concentrated on a rota-vapor, the residue was then partitioned between ethyl acetate (700 mL) and saturated sodium bicarbonate aqueous solution (500 mL). The organic phase was separated, washed with brine (2*200 mL), then dried over Na2SO4 and filtered. Evaporation of solvent gave the titled compound as an oil that was used in step B without further purification.

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-(4-Iodophenyl)butanoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Cano, Ivan Collado; Dominianni, Samuel James; Etgen, Garret Jay; Garcia-Paredes, Cristina; Johnston, Richard Duane; Letourneau, Michael Edward; Mantlo, Nathan Bryan; Martinelli, Michael John; Mayhugh, Daniel Ray; Saeed, Ashraf; Thompson, Richard Craig; Wang, Xiaodong; Coffey, David Scott; Schmid, Christopher Randall; Vicenzi, Jeffrey Thomas; Xu, Yanping; US2004/102500; (2004); 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. 58755-70-7, name is 1-Iodo-4-methoxy-2-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C7H6INO3

To a stirred solution of 4-iodo-3-nitroanisole (6.33 g, 22.7 mmol) in acetic acid (3.78 mL) and anhydrous EtOH (37.8 mL) were added Fe (7.60 g, 0.136 mol) and FeCl3 (2.21 g, 13.6 mmol) portionwise at room temperature, and then the mixture was heated to 80 C. After 40 min, the reaction mixture was filtered through a pad of Celite. To the resulting mixture was added H2O and the aqueous layer was extracted with EtOAc three times. The combined organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo. The residue was purified with flash column chromatography on silica gel (hexane/EtOAc=7/1) to afford 69 (4.77 g, 19.2 mmol, 84%) as a slightly yellow solid. Mp 33-34 C; IR (neat, cm-1) 3459, 3364, 2936, 1613, 1569, 1486, 1428, 1332; 1H NMR (CDCl3, 400 MHz) delta 7.47 (d, J=8.7 Hz, 1H), 6.32 (d, J=2.8 Hz, 1H), 6.13 (dd, J=8.7, 2.8 Hz, 1H), 4.06 (s, 2H), 3.74 (s, 3H); 13C NMR (CDCl3, 100 MHz) delta 161.1, 147.6, 139.2, 106.6, 100.5, 73.4, 55.3; HRMS (DART) calcd for C7H9INO ([M+H]+) 249.9729, found 249.9738.

The synthetic route of 58755-70-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yamakawa, Takayuki; Ideue, Eiji; Iwaki, Yuzo; Sato, Ayumu; Tokuyama, Hidetoshi; Shimokawa, Jun; Fukuyama, Tohru; Tetrahedron; vol. 67; 35; (2011); p. 6547 – 6560;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 181765-85-5, 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. 181765-85-5, name is Methyl 4-chloro-2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of methyl 4-chloro-2-iodobenzoate (5.93g, 20 mmol), 4-bromo-2-nitroaniline (4.34g, 20 mmol), copper (1.26g, 20 mmol), and K2CO3 (2.76g, 20 mmol) in chlorobenzene (300 mL) was heated to reflux for 2 days, cooled to room temperature, diluted with ethyl acetate, and filtered through diatomaceous earth (CELITE#). The solution was washed with water and brine, dried (MGS04), filtered, and concentrated under vacuum. The residue was purified by flash column chromatography on silica gel with 9: 1 hexanes/ethyl acetate to provide 6.86g (89 %) of the desired product. MS (DCI) m/e 386 (M+H) +, 403 (M+NH4) + ; 1H NMR (300 MHz, DMSO- D6) 8 10.83 (s, 1H), 8.28 (d, J = 2.4 Hz, 1H), 7.97 (d, J = 8.5 Hz, 1H), 7.82 (dd, J = 9.1, 2.4 Hz, 1H), 7.63 (d, J = 9. 1 HZ, 1H), 7.52 (d, J = 2. 1 HZ, 1H), 7.17 (dd, J = 8. 5, 2 Hz, 1H), 3.87 (s, 3H).

The synthetic route of Methyl 4-chloro-2-iodobenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBOTT LABORATORIES; WO2004/76424; (2004); A1;,
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. 167479-01-8, name is tert-Butyl (3-iodopropyl)carbamate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: tert-Butyl (3-iodopropyl)carbamate

Intermediate 7. A solution of glyoxal cyclen 1 (1.00 g, 5.15 mmol) and iert-butyl N-(3- iodopropyl)carbamate (1.64 g, 5.66 mmol) in 10 mL of dry THF was stirred for 4 days at room temperature. The resulting precipitate was recovered by filtration and washed with small portions of dry THF, to give a white solid (2.25 g, 91 % yield). ln NMR (D20, 300 MHz): 3.95-3.41 (m, 10H), 3.27-3.17 (m, 6H), 2.95-2.76 (m, 4H), 2.58-2.47 (m, 2H), 2.14-2.00 (m, 2H, CH^CHNHBoc), 1.44 (s, 9H, C(CH3. 13C NMR (D20, 300 MHz): 161.3 (CO), 87.1 (CHam), 84.6 (C(CH3)3), 75.0 (CHam), 65.3, 60.3, 9.3 (CH2NHCO), 54.5, 51.7, 51.4, 51.0, 50.9, 46.9, 40.3 (CHjNHCO), 31.1, 26.7 (CH^CH^HCO). HRMS (ESI): calculated for Ci8H34N502 [M+H]+: 352.270702; found: 352.270888.

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 167479-01-8.

Reference:
Patent; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE (CNRS); UNIVERSITE DE BRETAGNE OCCIDENTALE; OUKHATAR, Fatima; BEYLER, Maryline; TRIPIER, Raphael; (64 pag.)WO2016/87667; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 608-28-6,Some common heterocyclic compound, 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, molecular formula is C8H9I, 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.

Add 0.2 mmol of potassium carbonate,0.005 mmol of tris (dibenzylideneacetone) dipalladium,1,3-bis (diphenylphosphine) propane 0.02mmol,18-crown-6-ether 0.1mmol,1,3-dimethyl-2-iodobenzene 0.1 mmol,1-phenyl-1-butyne 0.25 mmol and N, N-dimethylformamide 1 mL were added toIn a 15 mL reaction tube, repeatedly fill 10 times with nitrogen, and stir at room temperature for 15 min.Add 0.5 mmol of water,Then placed in a reaction dish at 100 C for 16h; cooled to room temperature, the reaction solution was diluted with ethyl acetate, washed with water, the organic phase was dried over anhydrous Na2SO4, filtered, concentrated, and purified by thin layer chromatography to obtain 7.3mg of the target product. Color oil, 31% yield.

The synthetic route of 608-28-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (12 pag.)CN110256184; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 627-31-6, 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. 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip) belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Diiodopropane (0.295 g, 1.00 mmol, 5.0 eq) and potassium carbonate (0.028 g,0.20 mmol, 1.0 eq) were added to a solution of the phenol 33 (0.100 g, 0.020 mmol, 1.0 eq) in dry acetone (5 mL). The reaction mixture was heated at 60C for 6 hours when LC/MS showed complete reaction. The reaction mixture was concentrated to dryness under reduced pressure and the residue was purified by flash chromatography (silica gel,75/25 v/v n-hexane/EtOAc to 50/50 v/v n-hexane/EtOAc) to afford the product as acolourless oil (0.074 g, 56%). LC/MS (3.853 mm (ESj), m/z: 669.0 [M+H]. ?H NMR(400 MHz, CDC13) oe 7.26 (s, 1H), 6.90 (s, 1H), 6.68 (s, 1H), 6.24 (d, 1H, J = 15.3 Hz),5.87 (d, 1H, J= 8.9 Hz), 5.78 (m, 1H), 5.53 (m, 1H), 5.12 (m, 2H), 4.65 (m, 2H), 4.41 (m,1H), 4.11 (m, 1H), 3.93 (s, 3H), 3.81 (m, 1H), 3.40 (t, 2H, J 6.7 Hz), 3.05 (dd, 1H, J16.3, 10.1 Hz), 2.57 (m, 1H), 2.34 (m, 2H), 1.84 (d, 3H, J= 6.6 Hz), 0.92 (s, 9H), 0.28 (s,3H), 0.26 (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, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Reference:
Patent; STEM CENTRX, INC.; SPIROGEN SARL; TORGOV, Michael; HOWARD, Philip Wilson; WO2014/130879; (2014); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com