Month: July 2021

Synthetic Route of 444-29-1, A common heterocyclic compound, 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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.

Step-1: Synthesis of tert-butyl (Z)-(2-(4-(l-(4-(benzyloxy)phenyl)-2-(2- (trifluoromethyl)phenyl)but-l-en-l-yl)phenoxy)ethyl)carbamate 0 “C-RT/12 h Hi) l-iodo-2-(trifluoromethyl)benzene 4M KOH/80 °C/12 h To a stirred solution of l-(benzyloxy)-4-(but-l-yn-l-yl)benzene (2 g, 8.47 mmol, Example- 125, Step-4) in 2-methyl THF (20 mL), was added bis(pinacolato)diboron (2.15 g, 8.47 mmol), tetrakis(triphenylphosphine)platinum (0) (0.13 g, 0.104 mmol) under nitrogen atmosphere, reaction mixture was stirred at 90 °C for 12 h. The solution was allowed to cool to room temperature and tert-butyl (2-(4-iodophenoxy)ethyl)carbamate (2 g, 5.51 mmol), bis(triphenylphosphine)palladium (II) dichloride (0.276 g, 0.393 mmol), cesium carbonate (5.1 g, 15.74 mmol) and 2-methyl THF (20 mL) were added. This mixture was degassed with nitrogen and water (0.2 mL) was added. This mixture was stirred at room temperature for 12 h. After completion of reaction, to the above reaction mixture 4M KOH (11 mL, 4.48 mmol) and l-iodo-2-(trifluoiOmethyl)benzene (3.2 g, 12.2 mmol) were added. Reaction mixture was stirred at 80 °C for 12 h. After completion of reaction, reaction mixture was cooled to room temperature, diluted with water and extracted with EtOAc. The organic layer was dried over anhydrous sodium sulphate and concentrated under reduced pressure. The crude material was purified by column chromatography over 230-400 mesh silica gel using 5percent EtOAc in n- hexane to afford tert-butyl (Z)-(2-(4-(l-(4-(benzyloxy)phenyl)-2-(2- (trifluoromethyl)phenyl)but-l-en-l-yl)phenoxy)ethyl)carbamate (2 g, 36percent).

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EISAI R&D MANAGEMENT CO., LTD.; HAO, Ming-Hong; KORPAL, Manav; NYAVANANDI, Vijay Kumar; PUYANG, Xiaoling; SAMAJDAR, Susanta; SMITH, Peter Gerard; WANG, John; ZHENG, Guo Zhu; ZHU, Ping; (161 pag.)WO2016/196342; (2016); 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. 455-13-0, name is 4-Iodobenzotrifluoride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 4-Iodobenzotrifluoride

General procedure: A 25 mM solution of iodobenzene (5a) and K2CO3 (2 equiv) in H2O/CH3CN (2:1) was pumped at a flow rate of 1.0 mL/min(contact time: 58 s) through a Phoenix flow reactor systemequipped with two cartridges of 4 (total 500 mg; 0.084 mmolPd). Flow hydroxycarbonylation with CO gas introduced from agas module (10 mL/min) was conducted at 100 C and a systempressure of 5 bar. The resulting solution was collected for 50min (50 mL) and the solvent was removed by evaporation. 2 Naq HCl (10 mL) was added and the resulting solid was collectedby filtration, washed with H2O (3 × 10 mL), and dried undervacuum to give benzoic acid (9a) as a white solid without anyfurther purification.Yield: 125 mg (82%); mp 122 C; 1H NMR(400 MHz, DMSO-d6): delta = 12.96 (br s, 1 H, COOH), 7.93 (d, J = 7.2Hz, 2 H, PhH-2 and PhH-6), 7.62 (t, J = 7.2 Hz, 1 H, PhH-4), 7.49 (t, J =7.2 Hz, 2 H, PhH-3 and PhH-5); 13C NMR (101 MHz, DMSO-d6): delta = 167.32 (COOH), 132.87 (Ph), 130.76 (Ph), 129.26 (Ph),128.57 (Ph); ESI-TOF-MS (neg.): m/z = 121 [M – H]-.

The synthetic route of 455-13-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Osako, Takao; Kaiser, Reinhard; Torii, Kaoru; Uozumi, Yasuhiro; Synlett; vol. 30; 8; (2019); p. 961 – 966;,
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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., COA of Formula: C7H4F3IO

intermediate 13: step adiethyl 2-(4-(trifluoromethoxy)phenyl)malonateCul (0.26 g, 1.378 mmol), 2-picolinic acid (0.24 g, 1.969 mmol) and cesium carbonate (19.24 g, 59.061 mmol) were combined in a reaction vessel and the flask was evacuated and re-filled with argon (3 times). 1,4-Dioxane was then added followed by diethylmaionate (6 mL, 39.374 mmol) and l-iodo-4-(trifluoromethoxy)benzene (3 mL, 19.687 mmol). The resulting yellow suspension was stirred at room temperature for 48 hours and quenched with saturated NH4CI. The mixture was extracted with EtOAc (2x). The combined organic extracts were dried over Na2SQ4, filtered, and concentrated to provide the title compound.

The synthetic route of 103962-05-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BARBAY, Kent; EDWARDS, James, P.; KREUTTER, Kevin, D.; KUMMER, David, A.; MAHAROOF, Umar; NISHIMURA, Rachel; URBANSKI, Maud; VENKATESAN, Hariharan; WANG, Aihua; WOLIN, Ronald, L.; WOODS, Craig, R.; FOURIE, Anne; XUE, Xiaohua; CUMMINGS, Maxwell, D.; LEONARD, Kristi, A.; WO2015/57203; (2015); A1;,
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

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

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

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

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

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

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