Month: May 2021

Related Products of 52548-63-7, 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. 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step B: The product of Step A (9.0 g, 34 mmol) was dissolved in tetrahydrofuran (50 mL) and cooled in an ice bath under nitrogen. A 2.0 M solution of borane-methyl-sulfide complex (42 mL, 8.5 mmol) in tetrahydrofuran was added dropwise and the mixture was stirred for 30 minutes. The ice bath was removed and the reaction mixture was refluxed for 2 hours at 70 C. The solvent was concentrated in vacuo and the residue was dissolved in saturated ammonium chloride and extracted twice with methylene chloride. The organic extract was washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo to afford the desired product (6.2 g, 73%) as an off-white solid: 1H NMR (500 MHz, CDCl3) delta 7.78-7.69 (m, 1H), 7.31-7.22 (m, 1H), 6.83-6.75 (m, 1H), 4.64 (s, 2H), 2.04 (s, 1H).

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

Reference:
Patent; Molino, Bruce F.; Liu, Shuang; Guzzo, Peter R.; Beck, James P.; US2006/52378; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 2043-57-4, 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 2043-57-4 as follows.

Specifically, first, 2-(perfluorohexyl)ethyl iodide 21.70g (45.8mmol), 4-mercaptophenol 5.72 g (45.3 mmol), potassium carbonate 7.24 g (52.8 mmol), and put the acetone 50mL in 200mL eggplant flask, 2 days at 65 C, was reflux. After completion of the reaction was transferred to stand by separatory funnel to room temperature. There was separated ethyl acetate and brine after addition of the appropriate amount of water and 1N hydrochloric acid 30mL further added to the aqueous phase and an organic phase. Then, after standing for 30 minutes over anhydrous magnesium sulfate the organic phase, subjected to pleat folding filtered to obtain a filtrate was concentrated with an evaporator solid. The obtained solid was purified by silica gel column chromatography with chloroform to give Compound (A) 18.23g (38.6mmol). The obtained compound (A) is a colorless powder, whose melting point is 65 to 68 C, the yield was 85.2%. Further, an infrared spectrophotometer (manufactured by Shimadzu Corp., trade name “IRPrestige-21”. Similarly below. ), And nuclear magnetic resonance apparatus (Nippon Denshi Co. Ltd., trade name “JMN-LA500”. Similarly below. ) Was thus identified compound (A). The results are shown in the following.

According to the analysis of related databases, 2043-57-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; YAMAGUCHI UNIVERSITY; OKAMOTO, HIROAKI; MORITA, YUKI; (32 pag.)JP2016/64990; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 1829-28-3,Some common heterocyclic compound, 1829-28-3, name is Ethyl 2-iodobenzoate, molecular formula is C9H9IO2, 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 Procedures for Synthesis of 5-Aryl-2-Furaldehydes (5). 5-Aryl-2-furaldehyde 5 was synthesized from Suzuki coupling of 5-formyl-2-furanboronic acid and corresponding aryl halides 4 in 72-75percent yields following a literature procedure (Scheme 3) (Hosoya, et al. (2003) Bioorg. Med. Chem. 11:663). The crude solid products were purified by column chromatography using dichloromethane as eluent. wherein R2 is 2-NO2, 3,4-diMe (4a, 5a); H (4b, 5b); 4-NO2 (4c, 5c); 2-COOEt (4d, 5d).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 2-iodobenzoate, its application will become more common.

Reference:
Patent; Marmorstein, Ronen; Liu, Xin; Cole, Philip A.; Wang, Ling; Bowers, Erin M.; Meyers, David J.; Mukherjee, Chandrani; US2010/216853; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 364-77-2, name is 2-Iodo-5-fluoronitrobenzene, 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 364-77-2, SDS of cas: 364-77-2

General procedure: The appropriate 4-substituted-1-iodo-2-nitrobenzene 10 (1mmol), appropriate 1,3-disubstituted-5-aminopyrazole 11 (1.3mmol), and anhydrous potassium carbonate (248mg, 1.8mmol) were heated in the presence of rac-BINAP (23mg, 0.036mmol, 3.7mol%), Pd2dba3 (23mg, 0.024mmol, 2.5mol%), and 18-crown-6 (10mg, 0.038mmol) in toluene (8mL, purged with argon) at 100C. The reaction was carried out under argon for 24h. After cooling the reaction mixture was filtered and purified using column chromatography on aluminium oxide with toluene, or a toluene-ethyl acetate mixture (10:1) as an eluent. The product was recrystallized from toluene.

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-Iodo-5-fluoronitrobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Danel, Andrzej; Wojtasik, Katarzyna; Szlachcic, Pawe?; Gryl, Marlena; Stadnicka, Katarzyna; Tetrahedron; vol. 73; 34; (2017); p. 5072 – 5081;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, molecular formula is C7H4F3IO, 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 1-Iodo-4-(trifluoromethoxy)benzene

General procedure: Under argon, imidazo[2,1-c][1,2,4]triazine 1 (100mg, 0.44mmol), (hetero)aryl iodide (0.46mmol) and cesium carbonate (216mg, 0.66mmol) were solubilized in 2mL of toluene. The mixture was evacuated and back-filled with dry argon twice and Xantphos (26mg, 0.044mmol), Palladium acetate (5mg, 0.022mmol) were added and the mixture was submitted to reflux with stirring for 8h. Then cooled to room temperature and the mixture was filtered through celite and the organic phase was extracted three times with ethyl acetate, dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified by flash chromatography on silica (EtOAc/EP 2:8 to 3:7) to provide the desired product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 103962-05-6, its application will become more common.

Reference:
Article; Loubidi, Mohammed; Jouha, Jabrane; Tber, Zahira; Khouili, Mostafa; Suzenet, Franck; Akssira, Mohamed; Erdogan, Muemin Alper; Koese, Fadime Ayd?n; Dagc?, Taner; Armagan, Gueliz; Saso, Luciano; Guillaumet, Gerald; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 113 – 123;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 629-09-4, 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. 629-09-4, name is 1,6-Diiodohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Sodium methoxide (25 wt. %, 5.5 mL, 24.1 mmol) was added bysyringe to 20 (4.0 mL, 24.3 mmol) in DMF (10 mL) over 20 min. Thereaction solution was heated at 63 C for 17 h. After cooling to 0 C,the reaction solution was treated with 3:1 cold 0.5 M HCl/6 M NaCl(200 mL) and was extracted with EtOAc (2 150 mL, 50 mL). Theorganic extracts were washed with 1% NaHSO3 (150 mL), H2O(2 150 mL) and 6 M NaCl (100 mL), and solvent was removedby rotary evaporation. Flash column chromatography using 4%then 6% EtOAc/petroleum ether furnished 1.61 g of 2174 (28%) asa liquid: 1H NMR d 3.37 (t, J = 6.4 Hz, 2H), 3.33 (s, 3H), 3.19 (t,J = 7.0 Hz, 2H), 1.83 (quintet, J = 7.1 Hz, 2H), 1.54-1.62 (m, 2H),1.33-1.46 (m, 4H). 13C NMR d 72.78, 58.72, 33.58, 30.46, 29.57,25.26, 7.25. HRMS m/z calcd for C7H19INO, 260.0506 (M+NH4);found, 260.0515. Anal. Calcd for C7H15IO: C, 34.73; H, 6.25.Found: C, 34.44; H, 6.19.

The synthetic route of 1,6-Diiodohexane has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bergeron, Raymond J.; Bharti, Neelam; McManis, James S.; Wiegand, Jan; Bioorganic and Medicinal Chemistry; vol. 23; 17; (2015); p. 5954 – 5971;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 34270-90-1,Some common heterocyclic compound, 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, molecular formula is C4H8I2O, 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.

Sodium bis(trimethylsilyl)amide solution in THF (1M, 19.5 mL, 19.5 mmol) was added dropwise to a solution of 2-(4-bromo-2-methylphenyl)acetonitrile (3.75 g, 17.85 mmol) in THF (90 mL) at 0C. After stirring for 0.5 h, the cooling bath was removed and the reaction mixture was stirred at 20C for 0.5 h. l-Iodo-2-(2-iodoethoxy)ethane (2.8 mL, 19.67 mmol) was added dropwise. The reaction mixture was stirred for 0.5 h at 20C. Sodium bis(trimethylsilyl)amide solution in THF (1M, 19.5 mL, 19.5 mmol) was added dropwise. The reaction mixture was stirred for 18 h at 20C, then quenched with saturated aqueous ammonium chloride solution (25 mL) and diluted with water (25 mL). The aqueous layer was extracted with EtOAc (3 x 50 mL). The combined organic extracts were washed with brine (50 mL) and dried over sodium sulfate, then filtered and concentrated in vacuo. The resulting brown oil was separated by flash column chromatography on silica, using a gradient of fc/7-butyl methyl ether in heptane (0-25%), to afford the title compound (2.3 g, 45%) as a yellow solid. 6n (250 MHz, CDCb) 7.47- 7.36 (m, 2H), 7.16 (d, 8.4 Hz, 1H), 4.16-4.06 (m, 2H), 4.06-3.91 (m, 2H), 2.65 (s, 3H), 2.33-2.21 (m, 2H), 2.17-1.99 (m, 2H). HPLC-MS (method 9): [M+water]+ m/z 297 and 299, RT 1.80 minutes.

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

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

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. 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 1-Iodo-2-(2-iodoethoxy)ethane

To the mixture of sodium 2-nitrophenolate (0.5 g, 3.1 mmol) in DMF (2 mL), 1-iodo-2-(2-iodoethoxy)ethane (3 g, 9.3 mmol) is added at room temperature. The mixture is heated at 80C. for 1 hour. EtOAc (100 mL) is added at room temperature and the white precipitate is removed by filtration. The organic layer is washed with water, brine, dried (anhydrous Na2SO4) and concentrated under vacuum. The crude product is purified by silica gel column chromatography to give Compound 3 (0.9 g).

The synthetic route of 34270-90-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AAT Bioquest, Inc.; Diwu, Zhenjun; Guo, Haitao; Peng, Ruogu; Zhao, Qin; Liao, Jinfang; Liu, Feng; (99 pag.)US9810700; (2017); B1;,
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 3718-88-5 as follows. Quality Control of 3-Iodobenzylamine hydrochloride

65 mg (0.16 mmol) of (3aS,4R,6aR)-4-(2,6-dichloropurin-9-yl)-2,2-dimethyltetrahydrothieno[3,4-d][1,3]dioxole-4-carboxylic acid methyl amide from the aforementioned Experimental Example 10, 55 mg (0.20 mmol) of 3-iodobenzylamine hydrochloride, and 0.065 mL (0.46 mmol) of triethylamine were added to ethanol and stirred at ambient temperature for 3 days. The reaction mixture was distilled under reduced pressure to obtain a concentrate. The concentrate was purified by silica gel column chromatography using the eluant (hexane:ethyl acetate=1:1) to obtain 87 mg (yield: 90%) of (3aS,4R,6aR)-4-[2-chloro-6-(3-iodobenzylamino)purin-9-yl)]-2,2-dimethyltetrahydrothieno[3,4-d][1,3]dioxole-4-carboxylic acid methyl amide as a white foam. 1H-NMR(CDCl3) delta: 1.43 (s, 3H), 1.61 (s, 3H), 2.88 (d, 3H), 3.07 (d, 2H) 4.73 (br d, 2H), 5.09 (m, 1H), 6.11 (d, 1H), 6.49 (br s, 1H), 7.07 (t, 1H), 7.32 (d, 1H), 7.60 (d, 1H), 7.72 (s, 1H), 8.16 (s, 1H) UV (methanol): lambdamax 271 nm (pH 7).

According to the analysis of related databases, 3718-88-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Government of the United States of America, repres ented by The Secretary, Department of Health and; Ewha Womans University; US2005/256143; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 51839-15-7,Some common heterocyclic compound, 51839-15-7, name is Dimethyl 5-iodoisophthalate, molecular formula is C10H9IO4, 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 a solution of dimethyl 5-iodoisophthalate (500 mg, 1.56 mmol, 1.0 eq) inMeOH (20 mL) was added an aqueous 1 M NaOH solution (4.69 mL, 4.69 mmol,3.0 eq). After stirring at 40 C temperature for 18 h, the brown suspension was diluted with water (10mL) and acidified to pH 3 with aqueous 1M HCl solution. The aqueous layer was extracted withEtOAc (3 x 20 mL). Combined organic extracts were washed with brine (20 mL), dried overanhydrous Na2SO4 and evaporated under reduced pressure to yield product 18 as a yellowish solid(455 mg, 100% yield), which was used in subsequent step without purification. 1H-NMR spectrumwas identical to that from the literature.9

The synthetic route of 51839-15-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zogota, Rimants; Kinena, Linda; Withers-Martinez, Chrislaine; Blackman, Michael J.; Bobrovs, Raitis; Pantelejevs, Teodors; Kanepe-Lapsa, Iveta; Ozola, Vita; Jaudzems, Kristaps; Suna, Edgars; Jirgensons, Aigars; European Journal of Medicinal Chemistry; vol. 163; (2019); p. 344 – 352;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com