Month: August 2021

Electric Literature of 461-17-6, 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. 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a suspension of silver nitrite (9 g, 58.5 mmol) in diethyl ether (25 mL) at 0C was added a solution of 4-iodo-1, 1, 1-trifluorobutane, 15.02 (10 g, 42.0 mmol) in diethyl ether (25 mL) slowly through an addition funnel (approx. 15 min). The resulting mixture was vigorously stirred at 0C and warmed to rt. After 50 h, the solid material was filtered off through a celite pad. The resulting diethyl ether solution was concentrated in vacuo to give 15.03 as colorless oil, which was used 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, 1,1,1-Trifluoro-4-iodobutane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SCHERING CORPORATION; WO2005/85197; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, 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. Computed Properties of C8H6BrIO2

A mixture of methyl 5-bromo-2-iodobenzoate (3.849 g,11.259 mmol), phenanthren-1-ylboronic acid (4) (3 g,13.510 mmol), 2 M aqueous potassium carbonate (30 mL), and tetrakis(triphenylphosphine)palladium (0.651 g, 0.563 mmol) in THF (100 mL) and methanol (30 mL) was heated at reflux in a nitrogen atmosphere for 24 h. After the reaction mixture had been concentrated in vacuo, the resulting mixture was extracted with dichloromethane. The organic layer was washed with water and brine and dried using anhydrous sodium sulfate. The filtrate was concentrated in vacuo to give a crude mixture that was purified by column chromatography (SiO2, dichloromethane:hexane 1:4) to afford methyl 5-bromo-2-(phenanthren-1-yl)benzoate (3.5 g,8.945 mmol, 79%) as a white solid. 1H NMR (300 MHz, CDCl3): delta (ppm) 8.80 (d, J = 12.6 Hz, 2H), 8.22 (s, 1H), 7.88 (d, J = 7.8 Hz, 1H),7.77 (dd, J = 5.1, 1.8 Hz, 1H), 7.73-7.60 (m, 4H), 7.40 (dd, J = 7.8,1.5 Hz, 2H), 7.32 (d, J = 8.1 Hz, 1H), 3.41 (s, 3H). 13C NMR (75 MHz,CDCl3): delta (ppm) 166.4, 140.7, 139.0, 134.6, 133.5, 133.1, 131.7, 130.3,130.2, 130.0, 128.5, 127.2, 126.8, 126.7, 125.7, 123.9, 122.9, 122.4,121.5, 52.1. HR-Mass (EI+): calcd for C22H15BrO2 390.0255, found392.0257.

The synthetic route of Methyl 5-bromo-2-iodobenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Jeong, Seongjin; Hong, Jong-In; Dyes and Pigments; vol. 144; (2017); p. 9 – 16;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 260355-20-2 as follows. Safety of 1-Chloro-4-iodo-2-(trifluoromethyl)benzene

The 1-chloro-4-iodo-2-trifluoromethylbenzene (10 mmol) obtained in the reaction 1.2 was dissolved in 20 ml of toluene, and the system was sequentially added with isoxazol-4-amine (12 mmol), palladium acetate ( 0.5 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (12 mmol), 3 ml of triethylamine, stirred for 10 minutes,Add 10 ml of cesium carbonate (10 mmol) aqueous solution, and heat to 50 C for 4 hours. After the reaction is completed, add 20 ml of water to the system, stir for 20 minutes, separate the liquid, and dry the organic phase with anhydrous sodium sulfate. Column chromatography gave 2.2 g of yellow N-(4-chloro-3-trifluoromethylphenyl)-isoxazole-4-amine powder in a yield of 84%

According to the analysis of related databases, 260355-20-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Zhang Ruwei; Ge Baoyin; Jing Fan; (7 pag.)CN108432777; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, 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 40400-15-5, Recommanded Product: 2-(2-Iodophenyl)acetonitrile

General procedure: A tube was loaded with CuCl (50 mg, 0.50 mmol) and CsF (228 mg,1.50 mmol) and sealed with a rubber septum. Anhydrous acetonitrile (1 mL) was added and the mixture was cooled to 0 C. Diethyl [(trimethylsilyl)difluoromethyl]phosphonate (neat, 325 mg, 1.25 mmol) was added and the mixture was heated at 40C for 1 h, cooled to 0 C and stirred at this temperature for 1 h. Pd(PPh3)Cl2 (18 mg,0.025 mmol) was added followed by a solution of the corresponding iodoarene 1 (0.50 mmol) in MeCN (1 mL). The suspension was stirred for 16 h at 40C. The reaction mixture was diluted with diethyl ether(15 mL), the organic layer was washed with water (15 mL), Na2CO3 (concentrated solution, 15 mL), dried over Na2SO4, and solvents were carefully removed under vacuum. Reverse-phase chromatography (H2O/MeCN or MeOH, gradient: 9:1 to 0:1, rate: 1% MeCN or MeOH per minute) gave the product 2.

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-(2-Iodophenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ivanova, Maria V.; Besset, Tatiana; Pannecoucke, Xavier; Poisson, Thomas; Synthesis; vol. 50; 4; (2018); p. 778 – 784;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 34270-90-1, 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. 34270-90-1 name is 1-Iodo-2-(2-iodoethoxy)ethane, 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 solution of Intermediate 34 (2.60 g, 10.9 mmol) in DML (20 mL) was added sodium hydride (1.04 g, 21.7 mmol) at 0C. The reaction mixture was stirred at r.t. for 30 minutes, then l-iodo-2-(2-iodoethoxy)ethane (5.31 g, 16.3 mmol) was added. The reaction mixture was heated at 80C for 16 h, then poured into ice and extracted with EtOAc (3 x 100 mL). The combined organic layers were separated, washed with water (100 mL) and brine (100 mL), then dried over anhydrous Na2S04and concentrated in vacuo. The crude residue was purified by flash chromatography on silica (0-20% EtOAc in hexanes) to afford the title compound (2.00 g, 60%) as a yellow oil. 6n (400 MHz, DMSO-de) 1.06 (t, J7.09 Hz, 3H), 1.95-2.02 (m, 2H), 2.17-2.22 (m, 2H), 3.64-3.71 (m, 2H), 3.72-3.80 (m, 2H), 3.85 (s, 3H), 4.05 (q, J6.85 Hz, 2H), 7.66 (d, J8.80 Hz, 1H),7.75 (s, 1H), 7.83-7.88 (m, 1H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-2-(2-iodoethoxy)ethane, and friends who are interested can also refer to it.

Reference:
Patent; UCB BIOPHARMA SRL; BRACE, Gareth Neil; BROOKINGS, Daniel Christopher; FOULKES, Gregory; LECOMTE, Fabien Claude; (0 pag.)WO2020/11731; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 128140-82-9, name is 1-(Difluoromethoxy)-4-iodobenzene, 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 128140-82-9, Quality Control of 1-(Difluoromethoxy)-4-iodobenzene

Step a) 1-(Difluoromethoxy)-4-(phenylethynyl)benzene Into a mixture of ethynylbenzene (1.9 g, 18.5 mmol), 1-(difluoromethoxy)-4-iodobenzene (5 g, 18.5 mmol), N,N-dimethylformamide (35 mL), and triethylamine (12.8 mL, 92.6 mmol) was introduced anhydrous argon for 5 minutes. Then, copper(I) iodide (1.85 mmol, 351 mg) and dichlorobis(triphenylphosphine)palladium(II) (1.11, 0.71 g) were added into the mixture and the new mixture was stirred at 60 C. for 3 hours. The mixture cooled to room temperature, poured into water and extracted with ethyl ether. The organic extracts were dried over MgSO4. Evaporation and purification on silica gel (ISCO) using hexanes/EtOAc (100/1) as the eluding solvent, gave 1-(difluoromethoxy)-4-(phenylethynyl)benzene as a clear oil (3.45 g, 76% yield). MS m/e M+244; 1H NMR (400 MHz, DMSO-d6) delta 7.2 (d, J=8.78 Hz, 2H), 7.28-7.45 (m, 4H), 7.5-7.55 (m, 2H), 7.6 (d, J=7.78 Hz, 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, 1-(Difluoromethoxy)-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; WYETH; US2009/48320; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 59528-27-7, name is (4-Iodophenyl)methanamine hydrochloride, 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 59528-27-7, Computed Properties of C7H9ClIN

A mixture of (4-iodophenyl)methanamine hydrochloride (5.0 g, 18.55 mmol, 1.0 eq), (1S,2S)-N1,N2- dimethylcyclohexane-l,2-diamine (0.59 mL 3.71 mmol, 0.2 eq), Sodium ascorbate (368 mg, 1.86 mmol, 0.1 eq), Copper Iodide (530 mg, 2.78 mmol, 0.15 eq), Sodium azide (2.41 g, 37.1 mmol, 2.0 eq) , Et3N (3.11 mL, 22.26 mmol, 1.2 eq) and 2-(prop-2-yn-l-yloxy)tetrahydro- 2H-pyran (2.6 g, 18.55 mmol, 1.0 eq) in Methanol (50 mL) and water (12 mL) were purged with Nitrogen for 5 minutes and heated to 55 C for overnight. The reaction mixture was cooled to room temperature and filtered through 413 filter paper. Celite was added and the solvent was removed under reduced pressure and the residue was purified over silica gel (120 g) using dichloromethane/(methanol containing 12 % (v/v) aqueous ammonium hydroxide) as mobile phase. The concentration of (methanol containing 12 % (v/v) aqueous ammonium hydroxide) was gradually increased from 0 % to 6.25 % to afford (4-(4-(((tetrahydro-2H-pyran-2- yl)oxy)methyl)-1H-1,2,3-triazol-1-yl)phenyl)methanamine (15, 3.54 g, 66%) as a white solid. LCMS m/z: [M + H]+ Calcd for Ci5H2oN402 289.2; Found 289.2.

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-Iodophenyl)methanamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SIGILON THERAPEUTICS, INC.; SEWELL, Jered, A.; CARMONA, Guillaume; GONZALEZ, Francisco, Caballerro; HEIDEBRECHT, Richard; MILLER, Robert, James; OBERLI, Matthias, Alexander; PERITT, David; SMITH, Devyn, McKinley; VEISEH, Omid; WOTTON, Paul, Kevin; (182 pag.)WO2019/67766; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 452-79-9, 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. 452-79-9, name is 2-Fluoro-1-iodo-4-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 180 (5R)-7-(2-Fluoro-4-methylphenyl)-2-(trans-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-l- one H A mixture of (5R)-2-(fralphar°-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-l-one (20 mg, 0.00007 mol, this compound was prepared by using procedures analogous to those described in example 1, steps 1-5), 4-methyl-2-fluoro-l-iodobenzene (21 mg, 0.00009 mol), sodium tert-bvAoxide (9.98 mg, 0.000104 mol), 1,4,7,10,13,16-hexaoxacyclooctadecane (27.4 mg, 0.000104 mol) , 2-(di- tert-butylphosphino)biphenyl (0.8 mg, 0.000003 mol) , tris(diben2ylideneacetone)dipalladium(0) (1 mg, 0.000001 mol), in tert-butyl alcohol (1.0 mL, 0.010 mol) was stirred at rt for 18. The crude product was purified by prep-HPLC to afford the desired product. . LC-MS: 361.1 (MfH)+.

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-1-iodo-4-methylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; INCYTE CORPORATION; WO2006/53024; (2006); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 19094-56-5, The chemical industry reduces the impact on the environment during synthesis 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, I believe this compound will play a more active role in future production and life.

EXAMPLE 57A A solution of 2-chloro-5-iodobenzoic acid (600 mg), phenylboronic acid (285 mg) and PdCl2(dppf) (173 mg) in 3M Na2CO3 (2.83 mL) and dioxane (4.5 mL) at 60 C. was stirred for 4 hours, cooled, acidified with 1M HCl, and extracted with ethyl acetate. The extract was washed with brine and concentrated. The concentrate was flash chromatographed on silica gel with ethyl acetate.

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-Chloro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wendt, Michael D.; Sun, Chaohong; Sauer, Daryl R.; Elmore, Steven W.; Kunzer, Aaron R.; US2007/72833; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 199850-56-1, The chemical industry reduces the impact on the environment during synthesis 199850-56-1, name is Methyl 2-amino-4-chloro-5-iodobenzoate, I believe this compound will play a more active role in future production and life.

Intermediate 11 1 : 7-Chloro-4-hvdroxy-6-iodo-3-(o-tolyloxy)quinolin-2(1 H)-oneMethyl 2-amino-4-chloro-5-iodobenzoate (Intermediate 2) (1 g, 3.21 mmol) and ethyl 2-(o- tolyloxy)acetate (Aldrich, 0.655 g, 3.37 mmol) were dissolved in THF (10 mL) and KHMDS 1 M/THF (9.63 mL, 9.63 mmol) was added in one portion at room temperature under N2. The reaction mixture was stirred at room temperature for 1 h before quenched with MeOH and concentrated under reduced pressure. The residue was dissolved in 1 N NaOH then extracted with Et20. The aqueous extracts were acidified with 1 N HCI and the resulting precipitate was collected by filtration then washed successively with water and diethyl ether to give 7-chloro-4-hydroxy-6-iodo-3-(o-tolyloxy)quinolin-2(1 H)-one (1.03 g, 2.409 mmol, 75 % yield) as white solid. LCMS: (M+H)+ = 428; Rt = 2.46 min.

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, Methyl 2-amino-4-chloro-5-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXOSMITHKLINE LLC; DAUGAN, Alain Claude-Marie; LAMOTTE, Yann; MIRGUET, Olivier; WO2012/119978; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com