Tag: M.W=200-300

Related Products of 660-49-1, A common heterocyclic compound, 660-49-1, name is 3-Fluoro-5-iodoaniline, molecular formula is C6H5FIN, 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 solution of 3-fluoro-5-iodoaniline (250 mg, 1.055 mmol) and dihydro-2H- pyran-4(3H)-one (264 mg, 2.637 mmol) in methanol (5 mL) was charged into a 25 mL round bottom flask with a magnetic stir bar. Acetic acid (0.121 mL, 2.11 mmol) was added and the resulting solution was stirred for 30 minutes at room temperature. Sodium cyanoborohydride (133 mg, 2.11 mmol) was added, the resulting solution was stirred overnight at room temperature. The reaction was quenched with 10 mL 1M aqueous NaOH, stirred for 15 minutes. The solution was extracted with EtOAc (3 x 15 mL), the combined organic layers were washed with brine (15 mL), dried with MgS04, filtered, and evaporated under vaccuum. The crude product was dry loaded onto 3 g. silica and purified by column chromatography (ISCO normal phase, 24 g. gold column, 0-60% EtOAc/hexanes gradient) to isolate N-(3-fluoro-5-iodophenyl)tetrahydro-2H-pyran-4- amine (047) (208 mg, 0.648 mmol, 61%). 1H NMR (400 MHz, CDCb) d ppm 1.41 – 1.55 (m, 2 H) 1.95 – 2.09 (m, 2 H) 3.38 – 3.48 (m, 1 H) 3.53 (td, 7=11.61, 2.13 Hz, 2 H) 3.65 – 3.80 (m, 1 H) 4.02 (br d, 7=11.54 Hz, 2 H) 6.20 – 6.30 (m, 1 H) 6.73 (br d, 7=1.76 Hz, 2 H). LCMS: 322.6 [M+H]+.

The synthetic route of 660-49-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COOK, Andrew; REYNOLDS, Dominic; ZHONG, Cheng; BRAWN, Ryan; ELLERY, Shelby; SAMARAKOON, Thiwanka; LIU, Xiang; PRAJAPATI, Sudeep; SHEEHAN, Megan; LOWE, Jason T.; PALACINO, James; (378 pag.)WO2019/200100; (2019); A1;,
Iodide – Wikipedia,
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Related Products of 71838-16-9,Some common heterocyclic compound, 71838-16-9, name is 2-Bromo-1-iodo-4-methylbenzene, molecular formula is C7H6BrI, 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: Method B: To a 10 mL sealed vial was added Cu(OAc)2·H2O (20 mg, 0.1 mmol), N-methoxy-1H-pyrrole-2-carboxamide (14 mg, 0.1mmol), aryl halide (1.0 mmol), aminobenzenethiol (1.2 mmol), KOH (224 mg, 4.0 mmol), PEG-100 (2.0 g) and a magnetic stir bar. The reaction mixture was stirred in an oil bath preheated to 90 C for 15 h. After allowing the mixture to cool to room temperature, the reaction mixture was extracted with ethyl acetate (3 × 40 mL) and water (40 mL). The combined organic phases were washed with brine, dried overanhydrous Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel to afford 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 2-Bromo-1-iodo-4-methylbenzene, its application will become more common.

Reference:
Article; Huang, Manna; Hou, Jianying; Yang, Ruiqiao; Zhang, Liting; Zhu, Xinhai; Wan, Yiqian; Synthesis; vol. 46; 24; (2014); p. 3356 – 3364;,
Iodide – Wikipedia,
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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. 612-55-5, name is 2-Iodonaphthalene, A new synthetic method of this compound is introduced below., Formula: C10H7I

A mixture of 1,1-dibromo-1,2,2,2-tetrafluoroethane (260 mg), magnesium powder (50 mg) and tetrahydrofuran was added to a three-necked flask equipped with a stirrer and a condenser and replaced with nitrogen. 5 C After the reaction was stirred for 24 hours, the reaction was complete to obtain a solution of a trifluorovinylmagnesium complex. The solution was heated to 40 C and 2-iodonaphthalene (300 mg) and tetrakis (triphenylphosphine palladium) (11.5 mg) were added and the reaction was continued for 6 hours. The column was passed through n-hexane to give a colorless liquid, Yield 90%.

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; Beijing Yuji Science And Technology Co., Ltd.; Chen Chaohui; Jia Xiaoqing; Quan Hengdao; (5 pag.)CN106866355; (2017); A;,
Iodide – Wikipedia,
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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,
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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,
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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,
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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

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

Synthetic Route of 2468-56-6, 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 2468-56-6 as follows.

3) Synthesis of 6-trifluoroacetamido-1-hexyne To a solution of sodium hydride (60% oil, 2.55 g, 63.6 mol) in DMF (50 ml), trifluoroacetamide (8.99 g, 79.6 mmol) was added portionwise as about 10 portions with ice cooling. Subsequently, a solution of 6-iodo-1-hexyne (3.31 g, 15.9 mmol) in DMF (15 ml) was added to the reaction mixture. The reaction mixture was stirred at room temperature for four hours. The reaction mixture was added with saturated aqueous ammonium chloride (100 ml) and ether (100 ml) for extraction. The ether layer was dried over magnesium sulfate, and concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (eluent; hexane-ethyl acetate mixed solvent) to afford 2.0 g of 6-trifluoroacetamido-1-hexyne (yield; 65.4%). Melting point: 41.0-42.5 C. 1H-NMR (270 MHz, CDCl3) delta ppm: 1.53-1.80 (m, 4H, -CH2(CH2)2-), 1.98 (t, 1H, J=2.7 Hz, H-CC-), 2.26 (dt, 2H, J=2.5, 6.7 Hz, CC-CH2-), 3.41 (q, 2H, J=6.8 Hz, CH2-N), 6.48 (brs, 1H, NHTfa)

According to the analysis of related databases, 2468-56-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; The Institute of Physical and Chemical Research; US6265569; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 13329-40-3,Some common heterocyclic compound, 13329-40-3, name is 1-(4-Iodophenyl)ethanone, molecular formula is C8H7IO, 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.

Dissolving 20 g (81 mmol) of 4′-iodo acetophenone into 200 milliliter of acetic acid, and adding 12.8 g (81 mmol) of bromine while cooling with ice, stirred at the temperature of 15 C for 3 hours. After the color of bromine disappeared, adding water and separating the precipitated solids by filtration, thereby obtained 27 g of crude 2-bromo-4′-iodo acetophenone.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(4-Iodophenyl)ethanone, its application will become more common.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; EP1582516; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com