Tag: M.W=200-300

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

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

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

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

Some common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, molecular formula is C9H11I, 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. Computed Properties of C9H11I

A solution of Pd(PPh3)2Cl2 (0.26 g, 0.41 mmol), triethylamine (1.7 mL, 12.2 mmol), l-iodo-2-isopropylbenzene (1.0 g, 4.1 mmol), CuI (0.077 g, 0.41 mmol) and trimethylsilylacetylene (0.19 g, 0.81 mmol) in DMF (15 mL) was heated for 30 min at 80 0C. The resulting mixture was concentrated and purified by silica gel chromatography using hexanes to afford the title compound as yellow oil (0.85 g, 97%). [0154] 1H NMR (500 MHz, DMSO-J6): delta 0.23 (s, 9H), 1.20 (d, J = 7.0 Hz, 6H), 3.35 (qn, J = 6.9 Hz, IH), 7.17 (td, J = 7.3, 1.8 Hz, IH), 7.31-7.39 (m, 3H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 19099-54-8, its application will become more common.

Reference:
Patent; TARGEGEN INC.; WO2009/55674; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

26059-40-5, name is 2-(2-Iodophenyl)ethan-1-ol, 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. SDS of cas: 26059-40-5

2-(2-iodophenyl)ethanol 91 (4.85 g, 19.60 mmol) was dissolved in acetonitrile (60 mL) and IBX (16.0 g, 57.10 mmol) was added at room temperature. The mixture was stirred under reflux for 1 hour and then cooled to room temperature. The mixture was then filtered through a large cotton plug, and the filtrate was concentrated and purified through a silica plug. The crude aldehyde was obtained as oil and used without further purification. A THF (10 mL) solution of the aldehyde obtained above was added to a solution of 2-methyl-1-propenylmagnesium bromide (64 mL, 32 mmol, 0.5 M in THF) in THF (65 mL) at 0 C via cannula, over 40 minutes. The reaction was allowed to warm to room temperature and stirred overnight. The reaction was then diluted with hexanes, quenched with saturated NH4Cl and extracted with diethyl ether (3 x 50 mL). The combined extracts were dried over MgSO4 and purified via silica gel flash chromatography (EtOAc/hexanes) to give iodide 11 as oil (3.37 g, 57%, 2 steps).

The synthetic route of 26059-40-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fischer, Derek; Nguyen, Thong X.; Trzoss, Lynnie; Dakanali, Marianna; Theodorakis, Emmanuel A.; Tetrahedron Letters; vol. 52; 38; (2011); p. 4920 – 4923;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 52548-63-7, name is 5-Fluoro-2-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 52548-63-7, SDS of cas: 52548-63-7

A solution of 150 g of potassium hydroxide in 850 ml of water is treated with 47.5 ml of thiophenol at 55 C under a nitrogen atmosphere. The mixture is stirred for 15 minutes and subsequently treated with 1.9 g of copper powder and 207 g of 5-fluoro-2-iodo-benzoic acid. The mixture is heated under reflux for 7 hours, filtered while hot, cooled and acidified with concentrated hydrochloric acid. The precipitated product is filtered off, washed with water and dried. There is obtained 3-fluoro-6-(phenylthio)-benzoic acid which melts at 146-148 C.

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-Fluoro-2-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hoffmann-La Roche Inc.; US4006144; (1977); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 6937-34-4, The chemical industry reduces the impact on the environment during synthesis 6937-34-4, name is 3-Iodophthalic acid, I believe this compound will play a more active role in future production and life.

(a) 4-Iodoisobenzofuran-l,3-dione. A solution of 3- iodophthalic acid (5.00 g, 17 mmol, commercially available from Fluorchem Products, West Columbia, SC) and acetic anhydride (15 mL) was placed in a sealed flask and then heated in an oil bath at 1400C for 4 hours. The solution was cooled to room temperature, and then placed in an ice bath. The solids were collected by filtration, washed with cold ether, and dried under vacuum.

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, 3-Iodophthalic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AMGEN INC.; WO2008/130508; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 103962-05-6, 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 103962-05-6 as follows.

To a 250 mL reaction flask was added 3-bromo-1H-1,2,4-triazole (5 g, 33.8 mmol), CuI (0.644 g, 3.38 mmol) and Cs2CO3 (11.01 g, 33.8 mmol). The flask was evacuated/backfilled with nitrogen gas, and then DMSO (33.8 ml) and 1-iodo-4-(trifluoromethoxy)benzene (4.87 g, 16.90 mmol) were added. The reaction mixture was heated to 100° C. for 20 hours (h). The reaction was cooled to room temperature (RT), diluted with EtOAc and filtered through a plug of Celite®. The Celite® was further washed with EtOAc. Water was added to the combined organics, and the layers were separated. The aqueous phase was neutralized to pH 7, and further extracted with EtOAc. The combined organics were concentrated in vacuo. Purification via flash chromatography (silica/EtOAc/hexanes) yielded 3-bromo-1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazole as an off-white solid (3.78 g, 12.27 mmol, 72.6percent): mp 69-70° C.; 1H NMR (400 MHz, CDCl3) delta 8.44 (s, 1H), 7.70 (d, J=8.9 Hz, 2H), 7.38 (d, J=8.5 Hz, 2H); 19F NMR (376 MHz, CDCl3) delta ?58.04; EIMS m/z 307.

According to the analysis of related databases, 103962-05-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Dow AgroSciences LLC; GIAMPIETRO, Natalie C.; CROUSE, Gary D.; WHITEKER, Gregory T.; US2014/275563; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com