Category: iodides-buliding-blocks

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. 610-97-9, name is Methyl 2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 610-97-9

General procedure: A 50 cm3 Schlenk flask was charged with an ortho-substituted iodoarene(1¡Á10-3 mol), an amine (1.1-5¡Á10-3 mol), K2CO3(2¡Á10-3 mol), a catalyst (5¡Á10-6 mol), and a stirring bar. Next, 5cm3 of DMF was added. Under balloon pressure of CO, the reactionmixture was stirred at 100 C for 1-6 h. After the reaction, the Schlenkflask was cooled down, and the organic products were extracted with3¡Á7 cm3 of diethyl ether (3¡Á15 min with stirring) and then GCanalyzed with dodecane as the internal standard (0.076 cm3, 5.46¡Á10-4 mol). Each reaction was repeated minimum twice and the averagevalue from two experiments was reported. The difference between tworesults was below 5%.After the solvents were evaporated, the crude product was purifiedby flash chromatography on silica gel using hexane/ethyl acetate (10:4)as the eluent, and the corresponding N-substituted phthalimides wereobtained

The synthetic route of 610-97-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wojcik, Przemys?aw; Trzeciak, Anna M.; Applied Catalysis A: General; vol. 560; (2018); p. 73 – 83;,
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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 3-Chloro-4-iodoaniline

[00675] Example 6: 4-[(aminocarbonyl) amino]-1-(3-chloro-4- iodophenyl)-1 H-pyrazole-3-carboxamide; [00677] Step 1: Preparation of (2E)-2- [ (3-chloro-4- iodophenyl) hydrazono] -2-cyanoacetamide; [00679] A 250 mL 2-neck flask, flushed with N2, was charged with a stir bar and 3-chloro-4-lodoaniline (19.01 g, 75 mmol) and was then cooled in acetone/ice bath to 0C. To this was added conc. HCI (19 mL) dropwise at a rate that maintained the temperature below 5C. Water (60 mL) was added followed by a solution of sodium nitrite (5.175 g, 75 mmol) in water (15 mL) over a 5 min period. After 75 mins, a solution of sodium acetate trihydrate (30.62 g, 225 mmol) in water (75 mL) was added over a 5 min. period with the temperature maintained at 5C. The resultant yellowish slurry was then used as described in the following paragraph. [00680] To a well-stirred solution of cyanoacetamide (12.61 g, 150 mmol) in water (115 mL) and ethanol (75 mL) in a 500-mL round bottom flask was added a solution of acetate trihydrate (10.5 g, 75 mmol) in water (25 mL) and this mixture was cooled to-7C in an acetone/water bath. To this solution was added the slurry from the previous paragraph dropwise over a 70-minute period with the temperature maintained at 0C ( 2C) during the addition. After 2.5 h, the cold mixture was filtered and the solids washed with water (3 X 100 mL) and air-dried. These solids were washed with methanol (4 X 100 mL) and dried in vacuo to give a yellow solid. The methanol washes were concentrated, cooled, and filtered to provide additional product.’H NMR (DMSO-d6) : 5 11.750 (m, 1 H), 7.940 (m, 1 H), 7.860 (m, 1 H), 7.822 (m, 1 H), 7.550 (m, 1 H), 7.330 (m, 1 H). MS (ESI-) for CgH6CIIN40 m/z 347.0 (M-H) -.

The synthetic route of 135050-44-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHARMACIA CORPORATION; WO2005/37797; (2005); 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. 620-05-3, name is (Iodomethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 620-05-3

General procedure: Hexamethylenetetramine 1 (70.1 mg), SDS (3.4 mg) and lanthanum triflate (17.6 mg) were dissolved in water (0.5 mL). Then 1o (271 mg) was added to the flask. The mixture was refluxed for 4 h to complete the reaction, which was monitored by TLC. The reaction mixture was extracted with EtOAc three times and the combined organic phases were distilled under reduced pressure. The crude product was purifiedby column chromatography on silica gel using hexane: EtOAc (5 : 1) as eluent to give 3o, recrystallisation of which from EtOH gave white crystals, 147 mg (71%) (Table 3, entry 1).

The synthetic route of 620-05-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Xu, Wenhao; Su, Weike; Journal of Chemical Research; vol. 38; 12; (2014); p. 710 – 714;,
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. 56404-21-8, name is 1-Iodo-2,4-dimethyl-3-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C8H8INO2

A mixture of l-iodo-2,4-dimethyl-3-nitrobenzene [56404-21-8] (1.50 g, 5.41 mmol), methyl 2,2-difluoro-2-(fluorosulfonyl)acetate [680-15-9] (6.24 g, 32.5 mmol), Cul (1.24 g, 6.50 mmol) and DIPEA (0.70 g, 5.41 mmol) in anhydrous DMF (13.9 mL) was stirred at 80 C for 2 h. The mixture was poured out in water and the aqueous phase was extracted with Et20. The combined organic extracts were washed with brine, dried (MgS04), filtered and concentrated under reduced pressure. The crude mixture was purified by flash column chromatography (silica, pentane/Et20, gradient from 100:0 to 90:10) to afford I- 100 (840 mg, 71%) as a yellow oil.

The synthetic route of 56404-21-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BARTOLOME-NEBREDA, Jose Manuel; TRABANCO-SUAREZ, Andres, Avelino; LEENAERTS, Joseph, Elisabeth; OEHLRICH, Daniel; BUIJNSTERS, Peter Jacobus Johannes Antonius; MARTINEZ LAMENCA, Carolina; VELTER, Adriana, Ingrid; VAN ROOSBROECK, Yves, Emiel, Maria; (110 pag.)WO2019/243533; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

0.2 mmol of cesium carbonate, 0.01 mmol of palladium acetate, 0.02 mmol of triphenylphosphine,1,4-Dihydro-1,4-epoxy naphthalene 0.2 mmol, methyl 4-iodo-3-methylbenzoate 0.1 mmol,0.15 mmol of hexamethyldisilazide and 1 ml of N,N-dimethylformamide were added to a 15 ml reaction tube.Nitrogen was repeatedly filled 3 times, placed in an oil bath at 100 C, reacted for 12 h; cooled to room temperature,The reaction solution was diluted with ethyl acetate and washed with water three times.The organic phase is dried over anhydrous Na2SO4.Filtered, concentrated, and purified by column chromatography36.3 mg of target product, yield 83%

According to the analysis of related databases, 5471-81-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (13 pag.)CN108586519; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 16355-92-3,Some common heterocyclic compound, 16355-92-3, name is 1,10-Diiododecane, molecular formula is C10H20I2, 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.

2,2′-(4S,4’S)-8,8′-(decane-1,10-diylbis(oxy)bis(6-(4-chlorophenyl)-1-methyl- 4H-benzo[f][1,2,4]triazolo[4,3-a][1,4]diazepine-8,4-diyl))bis(N-ethylacetamide) [Example 11]: A suspension of 2-(4S)-6-(4-chlorophenyl)-8-hydroxy-1-methyl-4H- benzo[f][1,2,4]triazolo[4,3-a][1,4]diazepin-4-yl)-N-ethylacetamide (208 mg, 0.507 mmol) in acetonitrile (10 mL) was charged with K2CO3 (82 mg, 0.6 mmol) and 1,10-diiododecane (100 mg, 0.254 mmol) and the resulting mixture was heated at 80 oC for 12 h. After the completion of reaction, the reaction mixture was concentrated in vacuo and the residue was partitioned between DCM (20 mL) and H2O (10 mL) and separated. The aqueous layer was re-extracted with DCM (3 X 15 mL) and the combined organic fractions were dried over anhydrous Na2SO4, filtered and concentrated in vacuo resulting in a crude product which was purified by preparative HPLC to afford 30 mg, (12 % yield ) of the title compound as a white solid. 1H NMR (400 MHz, DMSO-d6): = 8.26- 8.15 (m, 2H), 7.78 (t, J = 8.8 Hz, 2H), 7.50- 7.31 (m, 10H), 6.89- 6.80 (m, 2H), 4.47- 4.40 (m, 2H) , 4.06 – 3.85 (m, 4H), 3.36- 3.05 (m, 8H), 2.52 (s, 6H), 1.80- 1.60 (m, 4H), 1.40- 1.21 (m, 12H), 1.06 (t, J = 7.2 Hz, 6H); MS (ES+): m/z = 958.65, 960.70 [M+H] +; LCMS: tR = 3.3 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,10-Diiododecane, its application will become more common.

Reference:
Patent; COFERON, INC.; ARNOLD, Lee, Daniel; FOREMAN, Kenneth, W.; JIN, Meizhong; WANNER, Jutta; WERNER, Douglas, S.; WO2015/81284; (2015); 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. 13194-68-8, name is 4-Iodo-2-methylaniline, A new synthetic method of this compound is introduced below., Quality Control of 4-Iodo-2-methylaniline

(a) Preparation of 4-Fluoro-2-(4-iodo-2-methyl-phenylamino)-benzoic acid To a stirred solution containing 3.16 g (0.0133 mol) of 2-amino-5-iodotoluene in 5 mL of tetrahydrofuran at -78 C. was added 10 mL (0.020 mol) of a 2.0 M lithium diisopropylamide in tetrahydrofuran/heptane/ethylbenzene (Aldrich) solution. The resulting green suspension was stirred vigorously for 15 minutes, after which time a solution of 1.00 g (0.00632 mol) of 2,4-difluorobenzoic acid in 10 mL of tetrahydrofuran was added. The reaction temperature was allowed to increase slowly to room temperature, at which temperature the mixture was stirred for 2 days. The reaction mixture was concentrated by evaporation of the solvent under reduced pressure. Aqueous HCl (10%) was added to the concentrate, and the solution was extracted with dichloromethane. The organic phase was dried (MgSO4) and then concentrated over a steambath to low volume (10 mL) and cooled to room temperature. The off-white fibers which formed were collected by vacuum filtration, rinsed with hexane, and dried in a vacuum-oven (76 C.; ca. 10 mm of Hg) to afford 1.10 g (47%) of the desired material; mp 224-229.5 C.; 1H NMR (400 MHz, DMSO): delta 9.72 (s, 1H), 7.97 (dd, 1H, J=7.0, 8.7 Hz), 7.70 (d, 1H, J=1.5 Hz), 7.57 (dd, 1H, J=8.4, 1.9 Hz), 7.17 (d, 1H, J=8.2 Hz), 6.61-6.53 (m, 2H), 2.18 (s, 3H); 13C NMR (100 MHz, DMSO): delta 169.87, 166.36 (d,JC-F=249.4 Hz), 150.11 (d, JC-F=11.4 Hz), 139.83, 138.49, 136.07, 135.26 (d,JC-F=11.5 Hz), 135.07, 125.60, 109.32, 104.98 (d, JC-F=21.1 Hz), 99.54 (d, JC-F=26.0 Hz), 89.43, 17.52; 19F NMR (376 MHz, DMSO): delta-104.00 to -104.07 (m); IR (KBr) 1670 (C=O stretch)cm-1; MS (CI) M+1=372. Analysis calculated for C14H11FINO2: C, 45.31; H, 2.99; N, 3.77. Found: C, 45.21; H, 2.77; N, 3.64.

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; Gowan, Richard Carleton; Sebolt-Leopold, Judith; US2004/171632; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 10297-05-9, name is 1-Chloro-4-iodobutane, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

(1) Preparation of 1-(4-chlorobutoxy)-4-iodobenzene To a solution of 4-iodophenol (1.0 g) in acetonitrile (10 mL), cesium carbonate (3.0 g) and 1-chloro-4-iodobutane (1.2 g) were added and the mixture was heated to 100¡ãC, at which it was stirred for 4 hours. The reaction mixture was cooled to room temperature and filtered to remove insoluble materials, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by NH-type silica gel column chromatography (eluding solvent: n-hexane:ethyl acetate = 7:3 to 1:1) to give the titled compound (1.4 g, 99percent) as a brown oil.

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 10297-05-9.

Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD; EP2221298; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 21740-00-1, name is 5-Bromo-2-iodobenzoic acid, 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 21740-00-1, Application In Synthesis of 5-Bromo-2-iodobenzoic acid

Concentrated H2S04 (10 mL) was added dropwise to the solution of 5- bromo-2-iodobenzoic acid (100 g, 305.89 mmol) in MeOH (800 mL). The mixture was refluxed for 16 hours and then concentrated. The residue was dissolved in ethyl acetate (1 L). The organic layer was washed with saturated NaHCO3 and brine (3 x 200 mL), dried over Na2SO4, filtered and concentrated to afford targetproduct 5-Bromo-2-iodo-benzoic acid methyl ester (101.4 g, yield 90%) as yellow solid.LC purity: 98.91 % (254 nm); Mass: find peak 341 (M + H)+ at 2.214 mm.

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; SANOFI; PASCAL, Cecile; PELLET, Alain; COURTEMANCHE, Gilles; CAMPBELL, Simon; (78 pag.)WO2019/8027; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 116632-39-4, name is 5-Bromo-2-iodotoluene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 116632-39-4

Preparation 9 2-(2-Bromo-5-iodo-4-methylbenzyl) isoindoline-1,3-dione To a solution of 5-bromo-2-iodo toluene (512 mg, 1.72 mmol) in trifluoroacetic acid (5 mL) was added N-(hydroxymethy) phthalimide (305 mg, 1.72 mmol). The mixture developed a pink color. The solution was stirred at room temperature for 22 hours then concentrated sulfuric acid (1 mL) was added. The homogeneous solution was stirred for 18 hours at room temperature. Water was added and the precipitated solid collected by filtration and dried in a current of air (0.776 gm). This material, which by proton NMR analysis contained approximately 15% of an isomeric product, was carried forward to the following procedure without further purification. 1H NMR (400 MHz, CDCl3) delta7.85 (m, 2H) 7.76(m, 2H) 7.5 (s, 1H) 7.38(s, 1H) 4.84(s, 2H) 2.31(s, 3H). GC-MS calc. 455, found 455.

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 116632-39-4.

Reference:
Patent; Pfizer Inc; US2007/213371; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com