Month: July 2021

627-32-7, name is 3-Iodo-1-propanol, 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. COA of Formula: C3H7IO

The reaction of phenoxazine (500 mg, 2.729 mmol) and NaH (60% dispersion in mineral oil, 136.8 mg, 4.094 mmol) in distilled DMF (10 mL) with 3-bromo-1-propanol (621 mg, 4.094 mmol) ), as described above, gave compound 14 (480.7 mg, 1.992 mmol, 73 %) as dark navy oil.: Rf = 0.33 (n-hexane/EtOAc = 1:1); IR (neat, cm-1) 3365, 3065, 2947, 1592, 1487, 1380, 1272, 1130, 1044; 1H NMR (400 MHz, CD3OD) delta 6.72~6.76 (m, 2H), 6.51~6.61 (m, 6H), 3.66 (t, 2H, J = 5.6 Hz), 3.60 (t, 2H, J = 7.6 Hz), 1.80 (m, 2H); 13C NMR (100 MHz, CD3OD) delta 145.0, 133.4, 123.7, 120.6, 115.0, 111.6, 59.2, 40.5, 27.7; MS (FAB) m/z 241.1 (M+).

The synthetic route of 627-32-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gim, Hyo Jin; Li, Hua; Lee, Eun; Ryu, Jae-Ha; Jeon, Raok; Bioorganic and Medicinal Chemistry Letters; vol. 23; 2; (2013); p. 513 – 517;,
Iodide – Wikipedia,
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Synthetic Route of 124700-41-0, 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. 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The eighth compound (10.000 g, 37.592 mmol) was dissolved in 40 mL of dichloromethane and 1 mL of DMF, and stirred at room temperature. The oxalyl chloride (3.800 mL, 45.110 mmol) was dissolved in 10 mL of dichloromethane and added dropwise to the reaction system, and stirred at room temperature for 1 h. After the reaction is completed, the reaction solution is sparged.It was replaced with anhydrous toluene three times to obtain an oily liquid ninth compound.

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

Reference:
Patent; Beijing Institute of Technology; Liang Jianhua; Ma Congxuan; (36 pag.)CN109942653; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 5460-32-2, 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 5460-32-2 as follows.

In a 100 ml reaction flask equipped with an exhaust gas absorption device 2.64 g of 4-iodo-1,2-dimethoxybenzene and 26 ml of acetic acid, then add 30ml concentrated hydrochloric acid, control the reaction liquid temperature 15-20 degrees,dilute 10 ml of hydrogen peroxide diluted with 5 ml of glacial acetic acid, drop finished, dept at 15-25 degrees for 12 hours for sample HPLC monitoring, raw materials less than 1percent about 30 ml of saturated sodium bisulfite solution was added and filtered, the filter cake was transferred to a 100 ml reaction flask, 10 ml of acetic acid and 30 ml of water were added, The temperature was raised to 50-55 ° C for 1 hour, down to room temperature filtration, with a little water rinse, TLC test for a single spot. To give 3.04 white solid in 82percent yield. HPLC greater than 97.9 percent

According to the analysis of related databases, 5460-32-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Tianjin Chengjian University; GU, Ying-chun; FEI, Xue-ning; Ling, Big Yong; Li, Ran; JIAO, Xiu-mei; (6 pag.)CN105732333; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 4897-68-1, A common heterocyclic compound, 4897-68-1, name is 1-Bromo-2-iodo-4-methoxybenzene, molecular formula is C7H6BrIO, 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.

General procedure: In an oven dried Schlenk tube under nitrogen atmosphere, were added allylic alcohol 6 (500.0mg, 1.76-3.38mmol), aryl halide 1 (2.11-4.06mmol), Pd(OAc)2 (11.8-22.7mg, 3mol%), triethylamine (356.2-684.1mg, 3.52-6.76mmol), followed by dry acetonitrile (4mL), at room temperature. The resulted reaction mixture was stirred for 24h at 80C. Progress of the reaction was monitored by TLC. The reaction mixture was quenched with the aqueous NH4Cl solution and extracted with ethyl acetate (3×20mL). The organic layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure. Purification of the residue on a silica gel column chromatography using petroleum ether/ethyl acetate as eluent furnished the ketone 7 (46-58%).

The synthetic route of 4897-68-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ramulu, B. Venkat; Mahendar; Krishna; Reddy, A. Gopi Krishna; Suchand; Satyanarayana; Tetrahedron; vol. 69; 38; (2013); p. 8305 – 8315;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 19718-49-1,Some common heterocyclic compound, 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, molecular formula is C8H8INO2, 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 D: 4-Amino-N-(3,4-dimethoxyphenyl)-3-iodobenzamide A 500 mL round bottom flask was charged with methyl 4-amino-3-iodobenzoate (10.0 g, 36.1 mmol), methanol (270 mL), water (30 mL), and lithium hydroxide (1.82 g, 43.3 mmol). The vessel was flushed with nitrogen, fit with a reflux condenser, and the mixture heated to a gentle reflux for 20 h. The resulting mixture was then cooled to room temperature, acidify with 2N hydrochloric acid, then concentrated in vacuo. A 500 mL round bottom flask was charged with the resulting solid (9.5 g, 36.7 mmol) and dichloromethane (180 mL) was added. Bis(2-oxo-3-oxazolidinyl)phosphinic chloride (10.0 g, 39.5 mmol) and triethylamine (11.1 mL, 79.2 mmol) were added. 3,4-Dimethoxyaniline (11.1 g, 72.1 mmol) was then added and the resulting mixture was stirred at room temperature for 24 h. The resulting mixture was then diluted with ethyl acetate and washed with 1N NaOH. The organic layer was dried with MgSO4, filter, then concentrate in vacuo to yield 4-amino-N-(3,4-dimethoxyphenyl)-3-iodobenzamide. 1H NMR (300 MHz, CDCl3) delta 8.23 (s, 1 H), 7.73 (d, J=8.5 Hz, 1H), 7.42 (s, 1H), 7.30 (d, J=8.6 Hz, 1H), 6.90 (d, J=8.8 Hz, 1H), 6.77 (d, J=8.5 Hz, 1H), 3.74 (s, 3H), and 3.72 (s, 3H).

The synthetic route of 19718-49-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lawson, Edward C.; Hlasta, Dennis J.; Ghosh, Shyamali; DesJarlais, Renee L.; Schubert, Carsten; US2011/152321; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 127654-70-0, 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. 127654-70-0, name is 1-Chloro-3-fluoro-2-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

The compounds dibenzo[b,d]furan-2-ol (30g, 0.16mol), 1-chloro-3-fluoro-2-iodobenzene (41.7g, 0.16mol) in 300ml DMF in a nitrogen atmosphere completely After dissolving, potassium carbonate (44.2 g, 0.32 mol) was added and the mixture was heated with stirring for 2 hours. The temperature was lowered to room temperature, and water was added to obtain a solid, which was purified by column chromatography (chloroform / hexane) to give Compound 1-G (57.8 g, yield: 86%)

The chemical industry reduces the impact on the environment during synthesis 1-Chloro-3-fluoro-2-iodobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; LG Chem, Ltd.; Yoon Hong-sik; Hong Wan-pyo; Jeong Gyeong-seok; Kim Yeon-hwan; Yoon Hong-je; (49 pag.)KR2018/101265; (2018); A;,
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. 88-67-5, name is 2-Iodobenzoic acid, A new synthetic method of this compound is introduced below., SDS of cas: 88-67-5

Synthesized according to a slight modification of two previously reported procedures.18 Neat2-iodobenzoic acid (3.00 g, 12.1 mmol) was cooled down to 0 C, to which was added a mixture offuming HNO3 (3.0 mL) and concentrated H2SO4 (13.5 mL). This mixture was then stirred at 0 C for 1 h,then at rt for 30 min, and finally at 135 C for 2 h, before being cooled back down to rt. The resultingsolution was poured into plenty of ice water and filtered. The solid was transferred to an Erlenmeyer flaskand suspended in water (300 mL), then heated to a boil. A solution of KI (2.41 g, 14.5 mmol) in water (15mL) acidified to pH 3 with a few drops of concentrated H2SO4 was added portion-wise to this boiling suspension (I2 vapors were generated with each portion). Omitting this step as in Subramanian?s reportyields the iodoso analog. The solution was filtered while still boiling, then the filtrate was stored at 4 Cfor 18 h after which time the desired compound precipitated. 2-Iodo-5-nitrobenzoic acid was thencollected by filtration while still cold to afford 1.73 g (49%) as a 13:2 mixture with the undesired2-iodo-3-nitrobenzoic acid isomer. The inseparable mixture was used as is in the next step.Characterization matches the data previously reported in the literature

The synthetic route of 88-67-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Aubert-Nicol, Samuel; Heinrich, Nora; Lessard, Jean; Spino, Claude; Heterocycles; vol. 99; 1; (2019); p. 484 – 501;,
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. 16355-92-3, name is 1,10-Diiododecane, A new synthetic method of this compound is introduced below., Safety of 1,10-Diiododecane

EXAMPLE 22 N, N’-Decane-1, 10-diyl-bis-nicotinium Diiodide (bNDI).; S- (-)-Nicotine (30.8 mmol) was dissolved in glacial acetic acid (35 mL) and the solution was stirred at ambient temperature for 5 minutes. 1, 10-Diiododecane (15.4 mmol) was added to the solution and the mixture stirred and refluxed for 3 days. The mixture was then evaporated under reduced pressure to remove the solvent and the resulting oil was treated with an aqueous mixture of sodium bicarbonate. The aqueous mixture was extracted with ethyl ether (3 x 50 mL) and chloroform (3 x 50 mL) and the aqueous layer collected and was evaporated to dryness on a rotary evaporator, and the resulting solid was treated with chloroform and filtered. The filtrate was collected and evaporated to dryness. The resulting yellow oil was isolated in a 27% yield. ‘H NMR (300 MHz, CDC13) 8 9.55 (1H, s, C2-H), 9.44 (1H, d, C6-H), 8.53 (1H, d, C4-H), 8.09 (1H, m. C3-H), 4.98 (2H, t, C”1-CH2), 3.74 (1H, t, pyrolidine CH2), 3.30 (1H, t, pyrrolidine CH2,2. 50 (2H, m, C”2-CH2), 2.29 (3H, s, pyrrolidine N-CH3), 1.65-2. 20 (SH, m, pyrrolidine CH2CH2), 1.30-1. 57 (6H, m, C”3-5-CH2); 13C NMR (75 MHz, CDC13) 8 146.6, 143.9 x 2, 143.4, 128.4, 66.9, 61.9, 57.0, 40.8, 36.1, 32.1, 28.5, 28.2, 25.8, 23.5.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; UNIVERSITY OF KENTUCKY RESEARCH FOUNDATION; WO2005/66129; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 19094-56-5, 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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2-Chloro-5-iodobenzoic acid (10.0 g, 35.3 mmol) And suspended in methylene chloride (200 mL). N, N-Dimethylformamide (0.05 mL) was added to the resulting mixture, followed by the dropwise addition of oxalyl chloride (11.3 g, 89.0 mmol) at 0 C. After completion of the dropwise addition, the resulting mixture was allowed to warm to room temperature and stirred for 4 hours. The resulting clear solution was evaporated by rotary evaporation to remove the solvent and yielded 10.7 g of product in 100% yield, which was used directly in the next reaction without purification.

The synthetic route of 2-Chloro-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SENJU Pharma Corporation Limited; Woo, Frank; (28 pag.)KR2015/81220; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 58313-23-8, The chemical industry reduces the impact on the environment during synthesis 58313-23-8, name is Ethyl-3-iodobenzoate, I believe this compound will play a more active role in future production and life.

General procedure: To a dried sealed vessel was added 1,2,3,4-tetrahydroisoquinoline (5 mL, 40 mmol), anhydrous K2CO3 (8.34 g,60 mmol), CuI (0.8 g, 4 mmol), L-Proline (0.92 g, 8 mmol), ethyl 6-bromopicolinate (4.32 g, 20 mmol), and DMSO (25 mL). Then themixture was stirred at 80 C for 16 h under N2 environment. Aftercooling to room temperature, water (100 mL) was added andextracted with EtOAc. Then, the combined organic layer was driedover MgSO4, filtered, and concentrated. The residue was purified bysilica gel flash chromatography (hexane/EtOAc = 5/1) to providecompound 14 as a white oil (3.94 g, 70%).

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, Ethyl-3-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Fang, Yuying; Zhou, Huihao; Gu, Qiong; Xu, Jun; European Journal of Medicinal Chemistry; vol. 167; (2019); p. 133 – 145;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com