Author: Jessica.F

Adding a certain compound to certain chemical reactions, such as: 3930-83-4, name is 2-Iodobenzamide, 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 3930-83-4, Recommanded Product: 3930-83-4

General procedure: To a solution of 2-iodobenzamide (3) or 2-bromonicotinamide (6) (2.0 mmol) in DMSO (3 mL), was added aldehyde (2.2 mmol), NaN3 (260 mg, 4.0 mmol), CuBr (29 mg, 0.2 mmol), and l-proline (46 mg, 0.4 mmol). The reaction mixture was stirred at 80 C under air. After disappearance of the reactant (monitored by TLC), water (30 mL) was added to the mixture, and then extracted with ethyl acetate (15 mL) for three times. The extraction was washed with saturated NaCl solution, dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using petroleum ether/ethyl acetate (10:1 to 3:1) as the eluent to give the desired products 5 or 7.

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:
Article; Li, Ting; Chen, Minglu; Yang, Lei; Xiong, Zhengxin; Wang, Yongwei; Li, Fei; Chen, Dongyin; Tetrahedron; vol. 72; 6; (2016); p. 868 – 874;,
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. 181765-85-5, name is Methyl 4-chloro-2-iodobenzoate, A new synthetic method of this compound is introduced below., name: Methyl 4-chloro-2-iodobenzoate

Example 39Amethyl 2-(2-amino-4-(methoxycarbonyl)phenylamino)-4-chlorobenzoate To a solution of methyl-3,4-diaminobenzoate (2.8 g, 16.86 mmol, Alfa Aesar Chemical Company) in chlorobenzene (125 ml) was added Example 3A (5.0 g, 16.86 2345 mmol), K2CO3 (2.5 g, 17.71 mmol), and Cu (1.1 g, 16.86 mmol). The resulting mixture was heated at reflux over 18 hours. While hot, the mixture was filtered through a thin layer of diatomaceous earth and the cake washed with dichloromethane. The filtrate was concentrated and the crude product purified by flash chromatography on silica gel, eluting with a 10% – 100% CH2CI2 / hexanes gradient to yield the title compound. MS 2350 ESI(+) /M/Z 334.9 [M+H]+.

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; ABBOTT LABORATORIES; ABBOTT LABORATORIES TRADING(SHANGHAI) COMPANY, LTD.; VAN CAMP, Jennifer; PATEL, Jyoti, R.; SWANN, Steven; WO2012/45194; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 627-31-6, The chemical industry reduces the impact on the environment during synthesis 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), I believe this compound will play a more active role in future production and life.

General procedure: The mixture of 4-methylpiperazine-1-carbodithioate (2.21 gm, 11.16 mmol) and diiodomethane (0.3 mL, 3.72 mmol) in CH3CN (20 mL) was stirred at room temperature for overnight. The reaction mixture was concentrated under reduced pressure, crude product was treated with water (10 mL) and extracted with EtOAc (10 * 3 mL). EtOAc layer was washed with water (5 * 3 mL) and combined organic layers were dried on anhydrous sodium sulfate, filtered, and concentrated. The crude product was purified over column chromatography (100-200 mesh) using MeOH/CHCl3 as eluent to afford compound as white solid (0.76 g, 56%); 4.1.53 Propane-1,3-diyl bis(4-(3-cyanopropyl)piperazine-1-carbodithioate) (56) The title compound was synthesized from sodium 4-(3-cyanopropyl)piperazine-1-carbodithioate and diiodopropane in 56% yield as white solid; mp: 118-120 C; IR (KBr) nu (cm-1): 2942, 2823, 2248, 1646; 1H NMR (300 MHz, CDCl3 + CCl4): delta 4.34-4.05 (8H, m), 3.40 (4H, t, J = 7.1 Hz), 2.55-2.42 (16H, m), 2.16-2.07 (2H, m), 1.88-1.79 (4H, m); 13C NMR (75 MHz, CDCl3 + CCl4): delta 196.5 (C=S), 119.1, 55.9, 52.6, 50.7, 35.9, 28.2, 22.7, 15.0; ESI-MS: (m/z)499 (MH+); Anal. (%) calcd. for C21H34N6S4: C, 50.57; H, 6.87; N, 16.85; found C, 50.68; H, 6.94; N, 16.75.

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, 1,3-Diiodopropane(stabilized with Copper chip), other downstream synthetic routes, hurry up and to see.

Reference:
Article; Lal, Nand; Jangir, Santosh; Bala, Veenu; Mandalapu, Dhanaraju; Sarswat, Amit; Kumar, Lalit; Jain, Ashish; Kumar, Lokesh; Kushwaha, Bhavana; Pandey, Atindra K.; Krishna, Shagun; Rawat, Tara; Shukla, Praveen K.; Maikhuri, Jagdamba P.; Siddiqi, Mohammad I.; Gupta, Gopal; Sharma, Vishnu L.; European Journal of Medicinal Chemistry; vol. 115; (2016); p. 275 – 290;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 618-91-7, The chemical industry reduces the impact on the environment during synthesis 618-91-7, name is Methyl 3-iodobenzoate, I believe this compound will play a more active role in future production and life.

Intermediate 73a: Methyl 3-(3-hydroxyprop-1-yn-1-yl)benzoate Bis(triphenylphosphine)palladium(II) dichloride (0.67 g, 0.95 mmol) was added in one portion to methyl 3-iodobenzoate (5 g, 19.08 mmol) and copper(I) iodide (0.18 g, 0.95 mmol) in degassed THF (90 mL) at 20 C. under nitrogen. The resulting mixture was stirred for 5 minutes then prop-2-yn-1-ol (2.22 mL, 38.16 mmol) and triethylamine (5.31 mL, 38.16 mmol) was added. The reaction was stirred at 20 C. for 18 hours. The reaction mixture was diluted with EtOAc (200 mL), and washed sequentially with water (2*100 mL) and saturated brine (50 mL). The organic layer was dried with MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 50% EtOAc in heptane to afford the title compound (3.10 g, 85%) as a yellow solid; 1H NMR (400 MHz, CDCl3, 30 C.) 1.69 (1H, t), 3.92 (3H, s), 4.51 (2H, d), 7.40 (1H, t), 7.61 (1H, dt), 7.99 (1H, dt), 8.11 (1H, d).

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

Reference:
Patent; AstraZeneca AB; YANG, Bin; KETTLE, Jason Grant; HAYHOW, Thomas George Christopher; RASMUSSON, Timothy Gordon; NISSINK, Johannes Wilhelmus Maria; FALLAN, Charlene; Lamont, Gillian McGregor; (308 pag.)US2019/194190; (2019); 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. 249647-24-3, name is Methyl 3-bromo-4-iodobenzoate, A new synthetic method of this compound is introduced below., Formula: C8H6BrIO2

A solution of methyl 3-bromo-4-iodobenzoate (Preparation 23, 4.3 g, 12.6 mmol) in CH2Cl2 was cooled, under N2, to -78 C. DIBAL-H was added slowly to the solution, which was stirred at -78 C. for 45 minutes and then allowed to come to room temperature. Next, the reaction mixture was diluted with 1M HCL (40 mL) and stirred for 30 minutes. The reaction was further diluted with water and extracted with CH2Cl2. The organic phase was dried (Na2SO4) and concentrated under vacuum to afford the intermediate (3.2 g, 82%) as a solid. 1HNMR (CDCl3): 7.85 (1H), 7.67 (1H), 7.02 (1H), 4.65 (2H), 1.76 (1H, OH).

The synthetic route of 249647-24-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Vaillancourt, Valerie A.; Chubb, Nathan Anthony Logan; Curtis, Michael; Howson, William; Kyne, Graham M.; Menon, Sanjay; Sheehan, Susan M. K.; Skalitzky, Donald J.; Wendt, John A.; US2012/35122; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 2142-70-3, 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. 2142-70-3, name is 1-(2-Iodophenyl)ethanone belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A 10mL-sealed tube was charged with aryl iodides or bromides (1mmol), CuI (19mg, 0.1mmol), and DMEDA (13mg/16muL, 0.15mmol) in NH4OH (1.5mL, 27% NH3 in H2O) and DMSO (0.5mL). The tube was flushed with Ar gas before being capped. The solution was stirred for the given times at 130C or 110C. The resulting suspension was cooled to room temperature and saturated aqueous Na2SO4 solution (5mL) was added. The resulting solution was extracted with EtOAc (20mL×3). The organic layer was separated, dried over MgSO4, filtered and concentrated. The residue was purified by flash column chromatography (hexanes/EtOAc=5/1?1/2 or EtOAc) to give the desired primary arylamines.

The synthetic route of 1-(2-Iodophenyl)ethanone has been constantly updated, and we look forward to future research findings.

Reference:
Article; Jung, Hee Seon; Yun, Taeil; Cho, Yungyeong; Jeon, Heung Bae; Tetrahedron; vol. 72; 40; (2016); p. 5988 – 5993;,
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 199850-56-1 as follows. Product Details of 199850-56-1

General procedure: To a solution of methyl 2-amino-4-chlorobenzoate (300 mg, 1.6 mmol) and ethyl 2-phenoxyacetate (320 mg, 1.8 mmol) in anhydrous THF (9 mL) was added KHMDS (4.8 mL, 1.0 M in THF, 4.8 mmol) in one portion with vigorous stirring under a nitrogen atmosphere. The reaction mixture was stirred at rt until completion of the reaction (10 min) then MeOH was added. The reaction mixture was concentrated under reduced pressure and the resulting residue was taken up in water and acidified with 1 N HCl until precipitation occurred. The precipitate was filtered, washed with EtOH then dried to give 7-chloro-4-hydroxy-3-phenoxyquinolin-2(1H)-one (Table 2, entry 1) as a pale pink powder (449 mg, 92%).

According to the analysis of related databases, 199850-56-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Toum, Jerome; Moquette, Alexandre; Lamotte, Yann; Mirguet, Olivier; Tetrahedron Letters; vol. 53; 15; (2012); p. 1920 – 1923;,
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 25252-00-0 as follows. Recommanded Product: 25252-00-0

Tetrahydrofuran (99.7g) and sodium borohydride (15.2g, 0.4mol) were added to the reaction flask at 10-25C.A solution of 2-bromo-5-iodobenzoic acid (109.4 g, 0.34 mol, prepared in Example 2) in tetrahydrofuran (151 g) was slowly added dropwise.At 10-30C, a solution of sulfuric acid (16.4 g) in tetrahydrofuran (25 g) was added dropwise to the reaction vessel. After the addition was completed, the reaction was performed at room temperature for 2 hours. Then, it was heated to reflux 66C, refluxed for 2 hours, and then lowered to room temperature. 5% hydrochloric acid (235 g) was slowly added dropwise and THF was distilled off under reduced pressure (-0.01 MPa).Add 326.7 g of MTBE and 222.7 g of water to dissolve the solid, cool to 15-25C, separate the layers, and evaporate the organic layer under reduced pressure (-0.095 MPa).Toluene (108.8 g) and water (108.8 g) were added and the mixture was warmed to 60C for 1 h, reduced to 18-22C and filtered. After drying, 89.1 g of an off-white solid product was obtained with a measured content of >99% and a yield of 85.1%.

According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jinkai (Liaoning) Chemical Co., Ltd.; Wang Yongcan; Zhang Hong; Li Zhenwei; Zhao Yang; Zhang Guifang; Song Tongji; Hu Zhenzhu; Huang Fengting; (8 pag.)CN107954861; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 39998-81-7, 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. 39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation of 1-(2-fluoro-4-iodobenzyl)-4-ethyl-2-propyl-1H-imidazole-5-carboxaldehyde A solution of 2-fluoro-4-iodotoluene (47.28 g, 0.20 mol), N-bromosuccinamide (37.64 g, 0.21 mol) and azobisisobutyronitrile (3.65 g, 0.02 mol) in CCl4 (200 mL) was refluxed under N2 overnight. The mixture was cooled, the solid was filtered off and washed with CCl4. The filtrate was concentrated. The precipitated formed was filtered and washed with hexane to give 13.92 g of 86% pure benzyl bromide. The mother liquid was concentrated to give 48.88 g of 60% pure benzyl bromide. Both fractions were used without further purification in the next step. 4-Ethyl-2-propyl-1H-imidazole-5-carboxaldehyde (6.32 g, 38.0 mmol), potassium carbonate (10.57 g, 76.5 mmol), and 2-fluoro-4-iodobenzyl bromide (13.90 g of 86%, 38.0 mmol) were added together with 50 mL of DMF. The reaction mixture was stirred at room temperature overnight under N2. The solvent was removed in vacuo and the residue was partitioned between EtOAc and H2 O. The two layers were separated. The aqueous layer was extracted with EtOAc. The combined organic mixture was washed with H2 O and brine, dried over MgSO4 and concentrated. The crude product mixture was purified by flash chromatography (silica gel, 30-50% EtOAc/hexane) to yield 10.63 g orange oil (70%). MS m/e 401.0, [M+H]+; 1 H NMR (300 MHz, CDCl3): delta0.95 (t, 3H, CH3), 1.32 (t, 3H, CH3), 1.70 (m, 2H, CH2), 2.60 (m, 2H, CH2), 2.82 (q, 2H, CH2), 5.52 (s, 2H, CH2 Ar), 6.42 (t, 1H, ArH), 7.38 (d, 1H, ArH), 7.42 (d, 1H, ArH), 9.73 (s, 1H, CHO).

The synthetic route of 2-Fluoro-4-iodo-1-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The Du Pont Merck Pharmaceutical Company; US5395844; (1995); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 103962-05-6, The chemical industry reduces the impact on the environment during synthesis 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, I believe this compound will play a more active role in future production and life.

To a solution of compound 03-4-1 (5.30 g, 20.6 mmol, 1.0 eq) in toluene (150 mL) was added 1-iodo-4-(trifluoromethoxy)benzene (7.12 g, 24.7 mmol, 3.87 mL, 1.2 eq), K3PO4 (10.9 g, 51.5 mmol, 2.5 eq), (1S,2S)-N1,N2-dimethylcyclohexane-1,2-diamine (879.0 mg, 6.18 mmol, 0.3 eq) and CuI (392.3 mg, 2.06 mmol, 0.1 eq) under N2 protection. The mixture was stirred at 110 °C for 18 h, cooled to room temperature, quenched by addition of H2O (250 mL) at room temperature, and diluted with EtOAc (250 mL). The organic layer was separated, washed with brine (300 mL), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to give a residue. The residue was purified by column chromatography (SiO2) to give compound 03-4-2 (7.00 g, 81percent 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, 1-Iodo-4-(trifluoromethoxy)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; KYRAS THERAPEUTICS, INC.; VACCA, Joseph P.; LI, Dansu; (587 pag.)WO2017/96045; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com