Tag: M.W=300-400

25252-00-0, Adding some certain compound to certain chemical reactions, such as: 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, 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 25252-00-0.

To the solution of 2-bromo-5-iodo-benzoic acid (10 g, 31 mmol) in methanol (100 ml) was added thionyl chloride (5 ml, 68 mmol). The mixture was heated at 55C for 12 hours. The solvent and reagent were removed under reduced pressure and the mixture was diluted with EtOAc. The organic solution was washed with saturated sodium bicarbonate, water, and brine, and was dried with sodium sulfate. Concentration gave 2- bromo-5-iodo-benzoic acid methyl ester (10.5 g).

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 25252-00-0.

Reference:
Patent; GILEAD SCIENCES, INC.; GUO, Hongyan; KATO, Darryl; KIRSCHBERG, Thorsten, A.; LIU, Hongtao; LINK, John, O.; MITCHELL, Michael, L.; PARRISH, Jay, P.; SQUIRES, Neil; SUN, Jianyu; TAYLOR, James; BACON, Elizabeth, M.; CANALES, Eda; CHO, Aesop; KIM, Choung, U.; COTTELL, Jeromy, J.; DESAI, Manoj, C.; HALCOMB, Randall, L.; KRYGOWSKI, Evan, S.; LAZERWITH, Scott, E.; LIU, Qi; MACKMAN, Richard; PYUN, Hyung-Jung; SAUGIER, Joseph, H.; TRENKLE, James, D.; TSE, Winston, C.; VIVIAN, Randall, W.; SCHROEDER, Scott, D.; WATKINS, William, J.; XU, Lianhong; YANG, Zheng-Yu; KELLAR, Terry; SHENG, Xiaoning; CLARKE, Michael, O’Neil, Hanrahan; CHOU, Chien-hung; GRAUPE, Michael; JIN, Haolun; MCFADDEN, Ryan; MISH, Michael, R.; METOBO, Samuel, E.; PHILLIPS, Barton, W.; VENKATARAMANI, Chandrasekar; WO2010/132601; (2010); 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. 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, A new synthetic method of this compound is introduced below., 25252-00-0

Example I 4-Bromo-3-hydroxvmethyl- 1 iodo-benzeneOxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo5-iodo-benzoic acid (49.5 g) in CH2CI2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h Then the solution is concentrated under reduced pressure and the residue is dissolved in THE (100 mL). The resulting solution is cooled in an ice-bath andLiBH4 (3A g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2SO4) and the solvent is evaporated under reduced pressure to give the crude product.Yield: 47.0 g (99% of theory)

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; BOEHRINGER INGELHEIM VETMEDICA GMBH; ECKHARDT, Matthias; BUTZ, Tanja; HIMMELSBACH, Frank; MARTIN, Hans-Juergen; WO2014/16381; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

629-09-4, The chemical industry reduces the impact on the environment during synthesis 629-09-4, name is 1,6-Diiodohexane, I believe this compound will play a more active role in future production and life.

1,2-Dihydro-4-(6-iodohexyloxy)-1,2-dioxonaphthalene (5) A mixture of 1,6-diiodohexane (10.14 g, 30 mmol) and the silver salt of 2-hydroxy-1,4-naphthoquinone (2.81 g, 10 mmol) in benzene (60 mL) was stirred for 12 h at room temperature. The reacton mixture was filtered through Celite, concentrated in vacuo, and purified by flash chromatography (hexane/EtOAc 4:1) to give a yellow solid (2,19 g, 57%); mp 85-87 C.; 1H NMR (CDCl3) 8.12 (dd, J=6.5, 1.0 Hz, 1H), 7.86 (dd, J=6.9, 0.9 Hz, 1H), 7.70 (dt, J=7.6, 1.5 Hz, 1H), 7.58 (dt, J=7.5, 1.3 Hz, 1H), 5.95 (s, 1H), 4.15 (t, J=6.3, 2H), 3.22 (t, J=6.9 Hz, 2H), 1.80-2.05 (m, 4H), 1.45-2.10 (m, 4H).

The chemical industry reduces the impact on the environment during synthesis 1,6-Diiodohexane. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SLIL Biomedical Corporation; US6482943; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

672-57-1, Adding a certain compound to certain chemical reactions, such as: 672-57-1, name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, 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 672-57-1.

General procedure: To an oven-dry ground test tube equipped with a stir bar were added 1 mmol 2-bromoiodobenzene, 1mmolL-alaninamide, 3 mmol potassium carbonate and 5 mL DMF. The test tube was sealed with a rubber stopperand was evacuated and refilled with argon for three times. Then the test tube was stirred in an oil bathpreheated at 90? C for 48 hours. After the test tube was cooled to room temperature, the reaction wasquenched with water, and the reaction mixture was extracted with 20 mL ethyl acetate for three times. Thecombined organic layer was washed with 10 mL water and then saturated sodium chloride aqueous solution,and dried over anhydrous sodium sulfate. After filtration, the filtrate was condensed on a rotary evaporator invacuum. The resulting crude product was chromatographed on silica gel (300-400 mesh) with a 1:2 volumeratio mixed solution of ethyl acetate and petroleum ether as eluent to give a white solid L-N-phenylalaninamide.

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-Chloro-2-iodo-4-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wang, Yan; Tu, Xingzhao; Lv, Xirui; Zhou, Lihong; Zeng, Qingle; Tetrahedron Letters; vol. 54; 45; (2013); p. 6045 – 6048;,
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 162358-07-8 as follows. 162358-07-8

(2) Diethyl 2-acetamido-2-[2-(4-octylphenyl)ethyl]malonate To a suspension of sodium hydride (6 g) in dimethylformamide (100 ml), a solution of ethyl acetamidomalonate (33 g) in dimethylformamide (100 ml) was added under ice-cooling and the mixture was stirred at room temperature for 2 hours. A solution of 2-(4-octylphenyl)ethyl iodide (37 g) in dimethyl-formamide (100 ml) was added to the mixture under ice-cooling. The mixture was stirred for 2 hours at the same temperature and left standing overnight. The resultant mixture was poured into water and extracted with ethyl acetate. The extract was washed with a saturated brine and dried over magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel chromatography (eluent; hexane-ethyl acetate=3:1) to give the subject compound (25 g). Rf value: 0.40 (hexane-ethyl acetate=2:1) 1 H-NMR(400 MHz, CDCl:3) delta: 0.88 (3H, t, J=8 Hz), 1.20-1.30 (10H, m), 1.24 (6H, t, J=8 Hz), 1.50-1.62 (2H, m), 1.97 (3H, s), 2.45 (2H, dd, J=12, 8 Hz), 2.54 (2H, t, J=8 Hz), 2.68 (2H, dd, J=12, 8 Hz), 4.14-4.26 (4H, m), 6.75 (1H, s), 7.05 (2H, d, J=8 Hz), 7.08 (2H, d, J=8 Hz)

According to the analysis of related databases, 162358-07-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Yoshitomi Pharmaceutical Industries, Ltd.; US5948820; (1999); A;,
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. 25252-00-0, name is 2-Bromo-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 25252-00-0

Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid (49.5 g) in CH2CI2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and LiB (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2S04) and the solvent is evaporated under reduced pressure to give the crude product. Yield: 47.0 g (99% of theory)

The synthetic route of 25252-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM VETMEDICA GMBH; REICHE, Dania Birte; MOHREN, Nicole; JOHNSTON, Laura; SOMERVILLE, Bruce; VOTH, Rebecca K.; WO2015/150299; (2015); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 2043-55-2, name is 1,1,1,2,2,3,3,4,4-Nonafluoro-6-iodohexane, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 2043-55-2

Preparation of [CF3 (CF213CH2CH2LO-3H2] A mixture of 37.4 g of [1-IODO-LH, LH,] 2H, [2H-PERFLUOROHEXANE] and 50.0 g of triethyl phosphite was heated at [150 ¡ãC.] After 16 hr, an additional 50.0 g of triethyl phosphite was added, and heating was continued. After 2 hr, an additional 50.0 g of triethyl phosphite was again added, and heating was continued for another 24 hr. Diethyl ethylphosphonate and other volatiles were removed by distillation through a 12-inch (30 cm) vacuum- jacketed packed column, b. p. [34-38 ¡ãC] at 0.05 torr (7 Pa). Distillation of the concentrate provided 22.3 g of [1-DIETHYLPHOSPHONO-LH, LH,] 2H, 2H-perfluorohexane as a 90: 2: 7 mixture with triethyl phosphate and ethyl 1H, lH, 2H, 2H-perfluorohexyl ethylphosphonate as a clear, colorless liquid, b. p. [47-51 ¡ãC] at 0.05 torr (7 Pa).

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, 2043-55-2, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; 3M INNOVATIVE PROPERTIES COMPANY; WO2003/102003; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 672-57-1 name is 1-Chloro-2-iodo-4-(trifluoromethyl)benzene, 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. 672-57-1

General procedure: The corresponding iodobenzenederivative 14a or 14b (1.80 mmol) and 5-formyl furan-2-ylboronicacid 15 (2.34 mmol) were dissolvedin 10 mL DMF and 15 mL EtOH. The reaction mixture was stirred for 10 min underN2, then Pd(PPh3)2Cl2 (0.18 mmol)and a solution of Na2CO3 (2M, 10.8 mmol) were added to thereaction mixture, and the light-orange suspension was stirred under N2at room temperature. After 1 h the reaction went to completion (TLC) and wasquenched with 1M HCl, then EtOAc (10 mL) was added, and the mixture was stirreduntil the two layers became clear. The combined organic layers were washed withH2O and brine, dried over Na2SO4, filtered,and evaporated under reduced pressure. The crude product was purified by flashchromatography using PE/EtOAc as eluent to yield the desired product as a solid(yields: 8 (64%), 13 (87%)).

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

Reference:
Article; Botta, Lorenzo; Maccari, Giorgio; Calandro, Pierpaolo; Tiberi, Marika; Brai, Annalaura; Zamperini, Claudio; Canducci, Filippo; Chiariello, Mario; Marti-Centelles, Rosa; Falomir, Eva; Carda, Miguel; Bioorganic and Medicinal Chemistry Letters; vol. 27; 11; (2017); p. 2502 – 2505;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

112671-42-8, 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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In the round bottom flask, the benzo [b] thiophene-3- base boric acid (benzo[b]thiophen-3-ylboronicacid) 65.1g, 4-bromo-1-iodo-2-nitrobenzene (4-bromo-1-iodo-2-nitrobenzene) 100g dissolving in toluene 1600 ml and adding K2CO3(2M) 455 ml and Pd (PPh3)4(four (triphenylphosphine) palladium) 10.5g of the backflow after stirring. In TLC (thinlayerchromatography, thin layer chromatography) confirmed the reaction and the reaction is terminated after addition of water. The organic layer using EA and extraction (ethanol) of the pressure-reducing filter after the column to purify 84.5g intermediate 4′ -1 (the yield is 83%).

The synthetic route of 112671-42-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xian, hao wan; an, xianzhe; han, zheng you; jin, jin tai; li, ying zhen; (67 pag.)CN105473594; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

915095-86-2, 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. 915095-86-2, name is (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, This compound has unique chemical properties. The synthetic route is as follows.

5-iodo-2-chlorophenyl) (4-fluorophenyl) methanone (18.03 g, 50 mmo 1) was added DMF (90 mL), Ice bath slowly add sodium ethoxide (3.748,1. Eq), After adding the reaction at room temperature for 1.5 h, tlc (after the detection reaction is completed, Ice bath slowly add water (180mL), Stirring crystallization lh, Filter, The filter cake was washed with water (200 mL) Beat with ethanol (50 mL) Filtered and dried to give 16.72 g of the pale yellow solid of compound lib, Yield: 86.5percent Purity: 99.53percent.

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; Shanghai Pharmaceutical Industry Institute; China Pharmaceutical Industry Zongyuan; Ma Shuai; Zhou Weicheng; (7 pag.)CN106928040; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com