Tag: M.W=200-300

Synthetic Route of 31599-61-8, 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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

Charged 1-iodo-2,4-dimethylbenzene (10 grams, 43.09 mmol, MW: 232.06), 2-hexyldecan-1-ol (12.54 grams, 51.71 mmol, MW: 242.44), cesium carbonate, (21.23 grams, 64.62 mmol, MW: 328.5), 1,10-phenathroline (1.55 grams, 8.601 mmol, MW: 180.21), copper (1) iodide (0.840 grams, 4.307 mmol, MW: 195.01) and 100 ml dry xylene in 350 milliliter three necked round bottom flask. The reaction mixture was heated with stirring at 140 C. for 24 hours under nitrogen. The resulting suspension was cooled to room temperature and filtered through celite and alumina. The low boiling (xylene) component removed by rotary evaporator and high boiling component by air bath oven at 200 C. under high vacuum for 1 hour. The residue was purified by flask chromatography on silica gel with hexane. The final colorless product yielded 7.0 grams (47%). The product 13C NMR analysis suggests the formation of alkylarylther product. 13C NMR (CDCl3): 158.01, 137.65, 130.27, 128.24, 116.28, 111.19, 70.99, 37.91, 32.12, 31.61, 30.18, 29.85, 29.47, 26.97, 22.90, 20.10, 18.83, 14.19.

The chemical industry reduces the impact on the environment during synthesis 4-Iodo-1,2-dimethylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ExxonMobil Research and Engineering Company; Patil, Abhimanyu O.; Bodige, Satish; Luo, Shuji; Deighton, Shane; Oumar-Mahamat, Halou; (24 pag.)US2017/137734; (2017); A1;,
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3930-83-4, name is 2-Iodobenzamide, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Quality Control of 2-Iodobenzamide

General procedure: 2-Iodobenzamide 1a (1.0 equiv.), 2-aminoisovaleric acid 2a (3.0 equiv.), Cs2CO3 (3.0 equiv.) and GO/Fe3O4-CuI (Cu+ 0.03 equiv.) were added to DMSO/ethylene glycol (60:1, v/v) in a round bottom flask. The reaction was monitored by TLC. The product was purified by column chromatography with petroleum ether/ethyl acetate (3:1, v/v) to give pure white solid 3a.

The synthetic route of 3930-83-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kong, Lu-Lu; Fan, Li-Yan; Chinese Chemical Letters; vol. 27; 6; (2016); p. 827 – 831;,
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These common heterocyclic compound, 61272-76-2, name is 4-Fluoro-2-iodoaniline, 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. Recommanded Product: 61272-76-2

General procedure: To a cooled solution of KOt-Bu (3,7 g, 30 mmol) in DMF (50 mL) was added dropwise at ?60 °C a solution of the appropriate 2-iodoaniline (9.6 mmol) in DMF (3 mL) and the nitroarene (9.6mmol) in DMF (8 mL). The mixture was stirred at ?60 °C for 0.5h then the temperature was raised slowly to ?30 °C, and the reaction was continued for an additional 1 h, poured into sat.NH4Cl solution (200 mL) and extracted with EtOAc. The extract was washed with H2O, brine, and dried with Na2SO4. After evaporation,the crude product mixture was subjected to column chromatography (SiO2, hexane?toluene). For analytical data, seethe Supporting Information.

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

Reference:
Article; Trawczy?ski, Adam; Telega, Magdalena; Wrobel, Zbigniew; Synlett; vol. 26; 10; (2015); p. 1352 – 1356;,
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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, Product Details of 364-77-2

Step 1. Methyl trans-(4-Fluoro-2-nitro)cinnamate The title compound was prepared according to the procedure described in step 1 of Example 133 from 3-fluoro-6-iodonitrobenzene and methyl acrylate. 1H-NMR (CDCl3) delta: 8.67 (1H, d, 15.8 Hz), 7.78 (1H, dd, 8.07 Hz, 2.65 Hz), 7.68-7.63 (2H, m), 6.34 (1H, d, 15.8 Hz), 3.84 (3H, s).

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; Nakao, Kazunari; Stevens, Rodney William; Kawamura, Kiyoshi; Uchida, Chikara; Koike, Hiroki; Caron, Stephane; US6608070; (2003); B1;,
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Some common heterocyclic compound, 108078-14-4, name is 2-Iodo-3-methylbenzoic acid, molecular formula is C8H7IO2, 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. HPLC of Formula: C8H7IO2

General procedure: A mixture of 2-iodo-5-methylbenzoic acid (2a; 0.2 mmol, 1equiv), styrene 1a (0.8 mmol, 4 equiv) and NaHCO3 (0.26 mmol,1.3 equiv) in DMSO (4 mL) was put into a quartz reaction tube(10 mL). N2 was flowed in for 10 min, then the tube was sealed and exposed to illumination with a high-pressure mercury lamp at 300 nm wavelength for 6 h. Water (20 mL) was added tothe reaction system and the mixture was extracted with ethyl acetate (3 × 20 mL). The organic phase was washed with saturated salt water, dried with anhydrous sodium sulfate, and thecrude products were obtained under reduced pressure and concentration.The purified products were purified by silica gel column chromatography (PE/EtOAc, 10:1), and the product 7-methyl-3-phenylisochroman-1-one 3a (75%) was obtained as apale-yellow liquid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108078-14-4, its application will become more common.

Reference:
Article; Zhang, Xiao; Huang, Binbin; Yang, Chao; Xia, Wujiong; Synlett; vol. 29; 1; (2018); p. 131 – 135;,
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Adding a certain compound to certain chemical reactions, such as: 2265-91-0, name is 1,3-Difluoro-5-iodobenzene, 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 2265-91-0, name: 1,3-Difluoro-5-iodobenzene

In a nitrogen atmosphere, carbazole and potassium tert-butoxide powder were dissolved in 20 mL of anhydrous dimethyl sulfoxide solution, and after mixing well, the reaction temperature rose to 120 C. After the temperature was stabilized, The solution of 1-iodo-3,5-difluorobenzenein anhydrous dimethyl sulfoxide was heated to 140 C after the dropwise addition, and the reaction time was 2 hours. Among them, 1-iodo-3,5-difluorobenzene, carbazole, and tert-butanol The molar ratio of potassium is 1: 2.1: 2.1; the mixed solution is cooled to room temperature and extracted, dried, and rotary solvent is used to remove excess solvent to obtain a crude product. The crude product was separated and purified by column chromatography to obtain compound DCzB-I. The eluent was chloroform: n-hexane = 1: 10 (volume ratio), and the yield was 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-Difluoro-5-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Fuzhou University; Guo Zhiyong; Xiao Hui; Lou Yuheng; Han Mingxi; (11 pag.)CN110272379; (2019); A;,
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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;,
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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;,
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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;,
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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;,
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