Author: Jessica.F

Reference of 3718-88-5, The chemical industry reduces the impact on the environment during synthesis 3718-88-5, name is 3-Iodobenzylamine hydrochloride, I believe this compound will play a more active role in future production and life.

Dissolve 2,6-dichloro-9-cyclopentylpurine (620 mg, crude), 3-iodobenzylamine hydrochloride (810 mg, 3.00 mmol) and triethylamine (835 muL, 6.00 mmol) in dry ethanol (20 mL). Heat at reflux for 15 hours, cool, and filter the solid to give the title compound as a white solid (680 mg).1H-NMR (Me2SO-d6 + D2O, delta): 8.27 (s, 1H, purine H-8), 7.74 (s, 1H), 7.61 (d, 1H), 7.39 (d, 1H), 7.16 (t, 1H), 4.78 (m, 1H), 4.62 (bs, 2H), 2.15 (m, 2H), 1.90 (m, 4H), 1.70 (m, 2H); CIMS (NH3) 454 (MH+), 328.

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-Iodobenzylamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Aventis Pharmaceuticals Inc.; EP1056745; (2004); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 774608-49-0, A common heterocyclic compound, 774608-49-0, name is 4-Bromo-1-chloro-2-iodobenzene, molecular formula is C6H3BrClI, 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.

j00340j To a solution of 4-bromo-1-chloro-2-iodobenzene (0.30 g, 0.95 mmol), cyclopropylboronic acid (97 mg, 1.1 mmol), [1,1 ?-bis(diphenylphosphino)ferrocenej dichloropalladium(II) (39 mg, 0.047 mmol) in dioxane (6 mL) and water (2 mL) under nitrogen at room temperature was added potassium phosphate (0.76 g, 3.6 mmol). The reaction mixture was stirred at 70 C for 3 hours, then diluted with water (10 mL) and extracted with ethyl acetate (3 x 10 mL). The combined organic layers were washed with brine (2 xlO mL), dried over sodium sulfate, filtered and concentrated in vacuo to give compound B-34 (0.30 g, crude) as a yellow oil.

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; FORUM PHARMACEUTICALS, INC.; ACHARYA, Raksha; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; COOK, Andrew, Simon; HARRISON, Bryce, Alden; McRINER, Andrew, J.; (267 pag.)WO2017/69980; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 755027-18-0, 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. 755027-18-0 name is 1-Bromo-4-iodo-2-methoxybenzene, 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.

General procedure: To a degassed solution of 1-bromo-4-iodo-2-methoxybenzene (2.2 g, 7.03 mmol), (4-methoxy-2-nitrophenyl)boronic acid (2.1 g, 10.55 mmol) in DME (80 mL) was added Pd(Ph3P)4 (812 mg, 0.7 mmol) and CsF (2.4 g, 15.82 mmol) under nitrogen. The reaction was then heated to 70 C for 18 h. The reaction was then extracted with EtOAc and water. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified silica (gradient elution, 3-40% EtOAc/hexanes) to give the title compound (2.7 g, 99%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-4-iodo-2-methoxybenzene, and friends who are interested can also refer to it.

Reference:
Article; Rudd, Michael T.; McCauley, John A.; Romano, Joseph J.; Butcher, John W.; Bush, Kimberly; McIntyre, Charles J.; Nguyen, Kevin T.; Gilbert, Kevin F.; Lyle, Terry A.; Holloway, M. Katharine; Wan, Bang-Lin; Vacca, Joseph P.; Summa, Vincenzo; Harper, Steven; Rowley, Michael; Carroll, Steven S.; Burlein, Christine; Dimuzio, Jillian M.; Gates, Adam; Graham, Donald J.; Huang, Qian; Ludmerer, Steven W.; McClain, Stephanie; McHale, Carolyn; Stahlhut, Mark; Fandozzi, Christine; Taylor, Anne; Trainor, Nicole; Olsen, David B.; Liverton, Nigel J.; Bioorganic and Medicinal Chemistry Letters; vol. 22; 23; (2012); p. 7201 – 7206;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 17024-12-3, name is 9-Iodophenanthrene, 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 17024-12-3, SDS of cas: 17024-12-3

General procedure: Bis(triphenylphosphane)palladium(II)dichloride (14.2 mg,20.0 mmol, 2.00 mol%) and copper(I) iodide (7.62 mg, 40.0 mmol,4.00 mol%) were placed in a flame-dried 10 mL Schlenk tube with amagnetic stir bar under a nitrogen atmosphere and the Schlenktube was evacuated and flushed with nitrogen two more times.DME (3.0 mL) was added and the resulting yellow solution wasstirred for several minutes at rt. Aryl iodide 1 (1.00 mmol, 1.00equiv) and potassium carbonate (276 mg, 2.00 mmol, 2.00 equiv)were added and the vessel was closed and heated to 40 C. Ethylpropiolate (2) (198 mg, 2.00 mmol, 2.00 equiv) was dissolved inDME (0.95 mL) and added slowly over 21 h (1.0 mL syringe,0.50 mm/min feed rate). After complete addition, the syringe wasrinsed in the reaction mixture and stirring was continued for 1 h at40 C. Celite was added to the dark brown mixture and the solventwas removed under reduced pressure. For purification, chromatographyon silica gel was performed using manual flash techniqueor a Biotage SP4 flash purification system with eluents consisting ofn-hexane and EtOAc or acetone.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 9-Iodophenanthrene, and friends who are interested can also refer to it.

Reference:
Article; Goetzinger, Alissa C.; Michaelis, Carina S.; Mueller, Thomas J.J.; Dyes and Pigments; vol. 143; (2017); p. 308 – 316;,
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. 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-Amino-2,4,6-triiodoisophthalic acid

In step 1, the product formed after the reaction of the compound A and the iodine chloride is compound B, 100 g of the compound B and 150 g of phosphorus pentachloride are mixed in a vessel, the reaction temperature is controlled at about 30 degrees Celsius, and the reaction time is controlled at 40 minutes. After the reaction is completed, a small amount of a chlorinating agent needs to be added to the reaction vessel. The chlorinating agent may be hydrochloric acid, and about 20 g of hydrochloric acid is added. After reacting for 10 minutes, it is rinsed with water, and then filtered to obtain a compound C.

According to the analysis of related databases, 35453-19-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hubei Tianshu Pharmaceutical Co., Ltd.; Liu Yunlong; (12 pag.)CN109293526; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 19718-49-1, A common heterocyclic compound, 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, molecular formula is C8H8INO2, 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.

A combined suspension of methyl 4-amino-3-iodobenzoate (2.50 g, 9.02 mmol), copper (_) iodide (35 mg, 0.18 mmol), bis(triphenylphosphine)palladium(II) dichloride (127 mg, 0.18 mmol), and 1-ethynyl-4-methylbenzene (1.37 mL, 10.83 mmol) were stirred in toluene and TEA (1/1, 76 mL) at ambient temperature for overnight. The reaction solvent was evaporated under reduced pressure, and the residue was purified by column chromatography with hexane/ethyl acetate (5/1, v/v) to obtain the compound 44 as a white solid (2.39 g, quant. yield): 1H NMR (400 MHz, DMSO-d6) _ 7.81 (d, J = 2.0 Hz, 1H), 7.65 (dd, J = 8.7, 2.1 Hz, 1H), 7.56- 53 (m, 2H), 7.24- 7.21 (m, 2H), 6.76 (d, J = 8.7 Hz, 1H), 6.36 (s, 2H), 3.75 (s, 3H), 2.33 (s, 3H); 13C NMR (100 MHz, DMSO-d6) _ 165.7, 153.4, 138.2, 133.8, 131.4, 131.0, 129.2, 119.6, 116.2, 113.2, 105.1, 94.4, 84.9, 51.5, 21.1.

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

Reference:
Patent; BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM; DALBY, Kevin N.; EDUPUGANTI, Ramakrishna; TALIAFERRO, Juliana; LEE, Juhyeon; (0 pag.)WO2018/160967; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 31827-94-8, The chemical industry reduces the impact on the environment during synthesis 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, I believe this compound will play a more active role in future production and life.

General procedure: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

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-Bromo-1-(4-iodophenyl)ethanone, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Secci, Daniela; Bizzarri, Bruna; Bolasco, Adriana; Carradori, Simone; D’Ascenzio, Melissa; Rivanera, Daniela; Mari, Emanuela; Polletta, Lucia; Zicari, Alessandra; European Journal of Medicinal Chemistry; vol. 53; (2012); p. 246 – 253;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, 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 355-43-1, Formula: C6F13I

Microreactor> [0213] The microreactor used in present Test Example is, as shown in FIG. 3, constituted with T-shaped micromixers (M1, M2), micro tube reactors (R1, R2), and tube reactors (P1, P2, P3) for precooling. [0214] For both of the micromixer M1 and the micromixer M2, T-shaped micromixers (micromixers 1 and 2, manufactured by Sankoh Seiki Kogyo Co., Ltd., inner diameter: 250 mum or 500 mum, see FIG. 3) were used. For the micro tube reactors and the tube reactors for precooling, a stainless steel tube (outer diameter: 1/16 inch (1.58 mm), inner diameter: 1,000 mum) manufactured by GL Sciences Inc. was used. The residence time was regulated, not by changing the flow rate, but by changing the length of the stainless steel tube. By submerging the whole of the microreactor in a thermostatic bath, the reaction temperature was set at -78 C. [0215] The solutions to be introduced into the microreactor were prepared in the same manner as in Test Example 1 except that in Test Example 1, the concentrations of CF3(CF2)5Br and benzaldehyde were set at 0.20 M and 0.10 M, respectively, and a 0.72 M n-butyllithium solution was prepared by diluting n-butyllithium (manufactured by Kanto Chemical Co., Inc.) with hexane. [0216] Into the T-shaped mixer M1, the mixed solution of CF3(CF2)5Br and benzaldehyde and the n-butyllithium solution were liquid-transferred at the flow rates of 6.00 mL/min and 1.50 mL/min, respectively, by using syringe pumps. The solutions were mixed in the micromixer M1, and were allowed to undergo continuous reaction in the tube reactor. Methanol (manufactured by Wako Pure Chemical Industries, Ltd.) was introduced from one inlet of the microreactor M2. In the micromixer M2, by mixing the reactants and the methanol with each other, methanol quenching was performed (see FIG. 3). [0217] The residence time in the tube reactor R1 (inner diameter: 1,000 mum, length: 12.5 cm) was set at 0.785 sec. [0218] The mixed reaction solution was discarded for a few minutes until the reaction was stabilized and then taken into a sampling tube for 30 sec. [0219] The yield of the fluorine-containing substituted compound was measured in the same manner as in Test Example 1. The result thus obtained is shown in Table 2.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, and friends who are interested can also refer to it.

Reference:
Patent; Taiyo Nippon Sanso Corporation; Kyoto University; YOSHIDA, Junichi; NAGAKI, Aiichiro; US2014/12027; (2014); A1;,
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. 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, A new synthetic method of this compound is introduced below., Formula: C8H7IO2

2-(2H-l,2,3-Triazol-2-vD-5-methylbenzoic acid (1-7)A solution of 2-iodo-5-methylbenzoic acid (4.0 g, 15.3 mmol) in DMF (10 mL) was treated with 1,2,3-triazole (2.1 g, 30.5 mmol), CsCO3 (9.95 g, 30.5 mmol), CuI (0.145 g, 0.76 mmol) and trans-N,N’-dimethylcyclohexane-l,2-diamine (0.43 g, 3.05 mmol). The mixture was heated at 120 0C for 10 min in a microwave reactor. The reaction was cooled to room temperature, diluted with water, and washed with EtOAc. The aqueous phase was acidified with IN HCl and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by gradient elution on SiO2 (0 to 10% MeOH in water with 0.1% AcOH) to give the faster eluting 2-(2H-l,2,3-triazol-2-yl)-5-methylbenzoic acid 1-5. followed by the undesired regioisomer isomer, l-(2H-l,2,3-triazol-2-yl)-5-methylbenzoic acid. Data for K7: 1HNMR (500 MHz, DMSO-d6) d 12.98 (br s , IH), 8.04 (s, 2H), 7.72-7.45 (m, 3H), 2.41 (s, 3H) ppm.

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; MERCK SHARP & DOHME CORP.; COX, Christopher, D.; FRALEY, Mark, E.; SCHREIER, John, D.; WO2010/48017; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 52548-14-8, name is 2-Iodo-5-methylbenzoic 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 52548-14-8, Formula: C8H7IO2

Step A: H2S04 95-98% (2.54 ml_, 0.048 mol) was added to a solution of 2-iodo-5- methylbenzoic acid (25.0 g, 0.095 mol) in MeOH (220 ml.) and refluxed for 20h. The rxn mixture was cooled with an ice bath, and 1 N aq. NaOH was added dropwise until pH 8 was reached. The org. solvent was removed in vacuo and the aq. layer was extracted with DCM (2x). The combined org. extracts were washed with sat. aq. NaHC03 (1 x) and H20 (1x), dried (Na2S04), filtered and concentrated in vacuo to give methyl 2-iodo-5-methylbenzoate as a pale yellow liquid which was used in the next step without further purification. LC-MS A: tR = 0.87 min; [M+H]+ = 259.22.

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; ACTELION PHARMACEUTICALS LTD; BOLLI, Martin; BOSS, Christoph; BROTSCHI, Christine; GUDE, Markus; HEIDMANN, Bibia; SIFFERLEN, Thierry; WILLIAMS, Jodi T.; WO2014/57435; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com