Category: iodides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 52914-23-5, name is 2-(4-Iodophenyl)ethanol, 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 52914-23-5, Formula: C8H9IO

D. 2-(4-Iodophenyl)ethylchloride To a 500 mL round-bottomed flask equipped with dropping funnel, condenser and N2 inlet were added 307 g (124 mmol) 2-(4-iodophenyl)ethanol, 200 mL chloroform, and 10.0 mL (124 mmol) pyridine. A solution of 13.5 mL (186 mmol) thionyl chloride in 50 mL chloroform was added dropwise over 15 min, and the reaction then heated at reflux for 2 hr. The reaction was cooled, the solvent evaporated, and the residue taken up in ethyl acetate, washed with 1 N hydrochloric acid, water, saturated aqueous sodium bicarbonate solution and brine, dried, and evaporated. The resulting oil was chromatographed on silica gel using 20% ethyl acetate in hexane as eluant to afford 32.6 g (99%) of the product as an oil. 1H-NMR (CDCl3, delta): 3.00 (t, J=7, 2H), 3.68 (t, J=7, 2H), 6.99 (m, 2H), 7.63 (m, 2H). 13C-NMR (CDCl3, delta): 38.6, 44.6, 92.3, 128.8, 130.9, 137.7.

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:
Patent; Pfizer Inc.; US6235747; (2001); B1;,
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. 1427311-76-9, name is (S)-1-(4-Iodo-5-methoxy-2-nitrophenyl)-2,2-dimethylpropan-1-ol, A new synthetic method of this compound is introduced below., COA of Formula: C12H16INO4

DMAP (463 mg, 3.80 mmol) and MsCl (177 mu?, 2.28 mmol) were added to a solution of compound 4 (400 mg, 0.76 mmol) in anhydrous CH2CI2 (5.0 mL) at 0C under a nitrogen atmosphere. The reaction was stirred at 0C for 10 mins and at room temperature for another 3 hours. The reaction was then diluted with CH2CI2 (20 mL). The solution was applied on a short silica gel plug (2 x 3 cm) and was eluted quickly with a hexane/ethyl acetate/triethylamine solvent system (80 mL, volume ratio: 80/20/0.5). The eluent was concentrated in vacuo, and the residue was mixed with (5)-l-(4-iodo-5-methoxy-2- nitrophenyl)-2,2-dimethyl-l-propanol (500 mg, 1.37 mmol). The mixture was heated at 115C for 45 min under a nitrogen atmosphere, cooled to room temperature and dissolved in THF (10 mL). w-Bu4NF (526 mg, 1.67 mmol) was added and the mixture was stirred at room temperature for 12 hours and then concentrated in vacuo. The residue was dissolved in CH2CI2 (50 mL) and washed with brine (50 mL), and the aqueous phase was extracted with CH2CI2 (20 mL) two times. The combined organic phase was dried over Na2S04, concentrated in vacuo, and the residue was purified by silica gel chromatography to yield 6- chloro-9-(P-D-2′-deoxyribofuranosyl)-7-[(5)-l-(4-iodo-5-methoxy-2-nitrophenyl)-2,2- dimethyl-propyloxy]-methyl-7-deazapurine 51 (135 mg, 29% for three steps). 1H NMR (400 MHz, CDCl3): delta 8.56 (s, 1 H, H-2), 8.21 (s, 1 H, Ph-H), 7.34 (s, 1 H, H-8), 7.02 (s, 1 H, Ph- H), 6.35 (dd, 1 H, J= 6.0 and 8.8 Hz, Eta-Gamma), 5.20 (s, 1 H, Ph-CH), 4.76 (dd, 2 H, J= 12.4 and 36.4 Hz, 7-CH2), 4.74 (m, 1 H, H-3′), 4.13 (m, 1 H, H-4′), 3.96 (m, 1 H, H-5’a), 3.92 (s, 3 H, OCH3), 3.80 (m, 1 H, H-5’b), 2.85 (m, 1 H, H-2’a), 2.30 (m, 1 H, H-2’b), 0.83 (s, 9 H, C(CH3)3).

The synthetic route of 1427311-76-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LASERGEN, INC.; STUPI, Brian, Philip; LI, Hong; WU, Weidong; HERSH, Megan, N.; HERTZOG, David; MORRIS, Sidney, E.; METZKER, Michael, L.; WO2013/40257; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 1542-34-3,Some common heterocyclic compound, 1542-34-3, name is 3,5-Difluoro-4-iodoaniline, molecular formula is C6H4F2IN, 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.

A suspension of 3,Sdifluoro4-4odoaniline (14.7 g, 55.9 mmol), CuT (0.745 g, 3.91 mmoi), bis(triphenyiphosphine)paiiadium(ll) dichioride (1 .59 g, 2,24 mrnoi), methyl 4 ethynylbenzoate (9.05 , 55.9 mmol), TEA (114 mL) and THF (44.1 mL) is stirred at 60Cfor 3 hr. The mixture is cooled to RT and the solvent evaporated to dryness under reduced pressure. EtOAc (10() mL) and H2() (100 mL) are added, and the resulting solid is filtered over diatornaceous earth. The organic layer from the filtrate is separated, dried over MgSO4, and evaporated to dryness under reduced pressure. A 1:1 mixture of DCM:heptane (400 nI) is added to the resulting residue and the mixture is stirred at RT overnight. The resultingsolid is collected by filtration and dried under vacuum to obtain the title compound (8.0 g,45.8% yield) as a brown solid. ?H NMR (300 MHz, DMSO-d6) oe 3.86 (s, 3H), 6.266.37 (m,4H), 7.59 (d, J = 8.2 Hz, 2H), 7.96 (d, J = 8.5 Hz, 2H).

The synthetic route of 1542-34-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; COATES, David Andrew; FALES, Kevin Robert; PETERSON, Jeffrey Alan; SCHKERYANTZ, Jeffrey Michael; SHEN, Quanrong; VALLI, Matthew John; WETTERAU II, John Rowley; WODKA, Dariusz Stanislaw; XU, Yangping; (118 pag.)WO2018/34883; (2018); 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. 3824-21-3, name is 2-Fluoro-4-iodo-1-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H6FIO

2-Fluoro-4-iodo-1-methoxybenzene a16 (0.0252 g, 0.10 mmol), acridine photosensitizer (A) (0.0029 g, 0.005 mmol) and L-valine were added sequentially under argon atmosphere. Ethyl b1 (0.0218 g, 0.15 mmol), 1,2-dichloroethane (DCE) 2.0 mL.The reaction was irradiated for 48 hours under a 6W blue light at room temperature.After completion of the reaction, the solvent was evaporated under reduced pressure and purified by column chromatography, eluting solvent: (V) petroleum ether / (V) ethyl acetate = 30/1.Yellow liquid (33) (0.0100 g, 87%) was obtained.

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 3824-21-3.

Reference:
Patent; Central China Normal University; Zhou Shaolin; Shi Weimin; (27 pag.)CN110294685; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 7212-28-4, name is 2-Iodo-N-phenylacetamide, 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. COA of Formula: C8H8INO

General procedure: 0.4 g (1.61 mmol) of 10, 1.93 mmol of 3a-j and 0.55 g (4.01 mmol) of K2CO3 were combined and refluxed in 20 ml acetone for 2 h. Then the solvent was reduced under reduced pressure. The crude product was washed with water, filtered and dried, followed by recrystallization from petroleum ether and ethyl acetate.

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

Reference:
Article; Liu, Wukun; Hua, Jie; Zhou, Jinpei; Zhang, Huibin; Zhu, Haiyang; Cheng, Yanhua; Gust, Ronald; Bioorganic and Medicinal Chemistry Letters; vol. 22; 15; (2012); p. 5008 – 5012;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 930599-57-8,Some common heterocyclic compound, 930599-57-8, name is 4-Iodo-2-methyl-1-(trifluoromethyl)benzene, molecular formula is C8H6F3I, 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.

To intermediate 164d (3.5 g, 12.24 mmol, 1.00 equiv) in CC14 (40 mL) at 60 C was added benzoyl peroxide (1.7 g, 7.02 mmol, 0.57 equiv) followed by the batch-wise addition of NBS (2.37 g, 13.32 mmol, 1.09 equiv) and the reaction stirred at reflux overnight. The solids were filtered out and the filtrate concentrated to afford 1.6 g (36%) of intermediate 164e as a red oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Iodo-2-methyl-1-(trifluoromethyl)benzene, its application will become more common.

Reference:
Patent; ARDELYX, INC.; LEWIS, Jason, G.; REICH, Nicholas; CHEN, Tao; JACOBS, Jeffrey W.; CHARMOT, Dominique; NAVRE, Marc; FINN, Patricia; CARRERAS, Christopher; SPENCER, Andrew; WO2013/96771; (2013); 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. 14192-12-2, name is 2,5-Diiodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2,5-Diiodobenzoic acid

To an oven-dried seal tube, was added 2,5-diiodobenzoic acid 6b (74.8 mg, 0.2 mmol), CuI (3.8 mg, 0.02 mmol) and K2CO3 (55.2 mg, 0.4 mmol). The reaction tube was evacuated and backfilled with argon. 2-Propanol (1.0 mL), ethylene glycol (22.3 muL) and thiol 5 (30 muL, 0.22 mmol) were added by syringes at room temperature. The tube was heated to 80 oC and stirred for 68 h. The reaction mixture was then allowed to reach room temperature. The reaction mixture was then filtered and concentrated in vacuo. The crude product was purified using CombiFlash automated chromatography system (methanol / methylene chloride, 0% to 10%) to afford the desired product 7b as white solid.

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 14192-12-2.

Reference:
Article; Zheng, Pinguan; Lieberman, Brian P.; Ploessl, Karl; Lemoine, Laetitia; Miller, Sara; Kung, Hank F.; Bioorganic and Medicinal Chemistry Letters; vol. 23; 3; (2013); p. 869 – 872;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 1309788-50-8, name is 3-Iodo-6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazole, 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. name: 3-Iodo-6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazole

Step 4: iert-Butyl 3-iodo-6,6-dimethyl-4,5,6,7-tetrahydro-lH-indazole-l-carboxylate: To a stirred solution of step 3 intermediate (3.9 g, 14.124 mmol) in dry tetrahydrofuran (20 ml), triethylamine (2.08 ml, 14.83 mmol), 4-dimethylaminopyridine (68 mg, 0.565 mmol) were added followed by addition of di-tert-butyl bicarbonate (3.23 g, 14.83 mmol) at room temperature and reaction mixture was stirred for 1 h at same temperature. The solvent was evaporated under reduced pressure and product was purified by column chromatography to yield 5.24 g of product as a pale yellow solid. 1H NMR (300 MHz, CDC13): delta 1.00 (s, 6H), 1.50 (t, / = 6.6 Hz, 2H), 1.59-1.69 (m, 9H), 2.31 (t, / = 6.3 Hz, 2H), 2.67 (s, 2H).

The synthetic route of 3-Iodo-6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; KUMAR, Sukeerthi; THOMAS, Abraham; KHAIRATKAR-JOSHI, Neelima; SHAH, Daisy Manish; WO2014/41518; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 1309788-50-8, name is 3-Iodo-6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazole, 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 1309788-50-8, SDS of cas: 1309788-50-8

To a solution of 3-iodo-6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazole (41 g, 147 mmol), triethylamine (22 ml, 155 mmol) and 4-dimethylaminopyridine (824 mg, 7 mmol) in tetrahydrofuran (163 ml) was added dropwise a solution of di-tert-butyl dicarbonate (34 g, 155 mmol) in tetrahydrofuran (41 ml) at room temperature over 40 min, and the mixture was stirred for 30 min. Then, the reaction mixture was is concentrated under reduced pressure. The residue was slurry-washed in hexane (130 ml) at 60 C. and ice-cooled. The crystals were collected by filtration, washed with hexane, and dried under reduced pressure to give the title compound (53 g, yield 95%).1H-NMR (400 MHz, DMSO-d6) delta: 0.95 (s, 6H), 1.46 (t, 2H, J=6.38 Hz), 1.56 (s, 9H), 2.23 (t, 2H, J=6.26 Hz), 2.63 (s, 2H).

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-Iodo-6,6-dimethyl-4,5,6,7-tetrahydro-1H-indazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; JAPAN TOBACCO INC.; US2011/306599; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 42048-11-3, name is 2-Chloro-6-iodotoluene, 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. Safety of 2-Chloro-6-iodotoluene

Under a protective atmosphere of inert gas, Pd(OAc)2 (2.2 mg, 10 mol%), XPhos (19.1 mg, 20 mol%), NBE-CO2K (3.5 mg, were added to a 4.0 mL reaction flask equipped with a magnetic stir bar. 10 mol%), 2-methyl-1-chloro-3-iodobenzene (0.2 mmol, 1.0 equiv.), ethylene oxide (0.6 mmol, 3.0 equiv.) and dry N-methylpyrrolidone(1.0 mL). The reaction flask was capped and stirred at room temperature for about 5 minutes, after which the mixture was heated to 80 C and stirred for 24 hours.After the reaction vessel was cooled to room temperature, it was quenched with water (10 mL), extracted with methyl tert-butyl ether (3×10 mL), dried over Na2SO4Filter and concentrate under vacuum. Purified by column chromatography, the eluent was petroleum ether: ethyl acetate = 20:1 (v/v) to afford 7-methyl-6-Chloro-2,3-dihydrobenzofuran 22 mg (yellow oily liquid, yield 64%).

The synthetic route of 2-Chloro-6-iodotoluene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wuhan University; Zhou Qianghui; Wu Chenggui; Cheng Honggang; (20 pag.)CN108329285; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com