Iodides-buliding-blocks

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. 459424-72-7, name is 1,2,3-Trifluoro-4-iodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 459424-72-7

To a solution of 1, 2, 3-trifluoro-4-iodobenzene (3.3 g, 18.8 mmoL) in 1, 4-dioxane (100 mL) was added 4, 4, 5, 5-tetramethyl-2- (1, 4-dioxaspiro [4.5] dec-7-en-8-yl) -1, 3, 2-dioxaborolane (5 g, 18.8 mmol) , Pd (dppf) Cl2(1.3 g, 1.88 mmol) and Cs2CO3(9.2 g, 28.2 mmol) and the mixture was heated at 70 for 5 hours. Then evaporated the solvent under reduced pressure and the residue was purified by column chromatography (PE: EA=5: 1) to give product as an oil (4.5 g in 88.6%yield) .

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; BEIGENE, LTD.; WANG, Hexiang; GUO, Yunhang; REN, Bo; WANG, Zhiwei; ZHANG, Guoliang; ZHOU, Changyou; (353 pag.)WO2018/54365; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 19231-06-2, name is Bis(4-methoxyphenyl)iodonium bromide, 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 19231-06-2, Recommanded Product: 19231-06-2

295 parts of the salt represented by the formula (I-17-a)88.25 parts of the compound represented by the formula (I-17-b) and 750 parts of chloroform,And the mixture was stirred at 23 C. for 1 hour.After concentrating the obtained reaction solution, to the obtained residue,1000 parts of tert-butyl methyl ether was added and stirred,By filtration, 328 parts of a salt represented by the formula (I-17-c) was obtained.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Bis(4-methoxyphenyl)iodonium bromide, and friends who are interested can also refer to it.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY LIMITED; ICHIKAWA, KOJI; FUJITA, SHINGO; ANRYU, YUKAKO; (69 pag.)JP6252292; (2017); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 404337-42-4, A common heterocyclic compound, 404337-42-4, name is 5-Chloro-2-iodo-m-xylene, molecular formula is C8H8ClI, 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.

To a 250 mL vessel equipped with a mechanical stirrer, thermometer, distillation head anddropping funnel, solid sodium hydroxide (3.9 g, 0.10 mol, microprills with 0.5- 1 mm diameter) is chargedunder an inert atmosphere.1-Methyl-2-pyrrolidone (NMP, 68 g) is added to the vessel in one portion through the dropping funnel and the reaction mixture cooled to 10 – 15 C while stirring. A solution of malononitrile (NEC-CH2- CEN) (2.27 g, 0.034 mol) in NMP (2.7 g) is added through the dropping funnel over 5 minutes maintainingthe temperature at 10 – 15 C. The reaction mixture is then heated to 100 C and a vacuum (30 mbar) applied, upon which solvent (32 g) is distilled off. The mixture is then heated to 130 C and a stream of nitrogen is passed through.2-lodo-5-chloro-1 ,3-dimethyl-benzene (9.0 g, 95% purity, 0.032 mol) is then added through the dropping funnel over 5 minutes at 130 CC. A mixture containing palladium (II) chloride (0.150 g, solutionin conc. hydrochloric acid, assay 20% Pd, 0.281 mmol), triphenylphosphine (0.186 g, 0.709 mmol) and NMP (13.7 g) is then added through the dropping funnel over a 2-minute period. The temperature is allowed to rise to 130 C and the reaction mixture stirred at this temperature for 80 mm. Conversion is monitored by pulling samples and subsequent HPLC analysis. A second portion of a mixture containing palladium (II) chloride (0.103 g, solution in conc. hydrochloric acid, assay 20% Pd, 0.194 mmol),triphenylphosphine (0.132 g, 0.504 mmol) and NMP (9.76 g) is then added through the dropping funnel over a 2-minute period and the reaction mixture stirred at 130 C for 40 mm.When conversion is complete, a vacuum (20 – 40 mbar) is applied and solvent (38 g) is distilled off. The resulting residue is cooled to 80 C and water (30 g) is added. After cooling to room temperature, the resulting mixture is filtered through a filter paper and the filter cake washed with water (10 g). To thecombined filtrates, hydrochloric acid (9.6 g, assay 32%, 0.084 mol) is added to adjust the pH from 13.3 to 1.3.The resulting mixture is extracted with toluene (50 g). The organic phase is washed with water (2 x 20g) and evaporated to dryness. The resulting solid residue is recrystallized from 1-pentanol (17 g) and the resulting crystals filtered, washed with 1-pentanol (4 g) and dried under vacuum to yield 2-(4-chloro-2,6-dimethyl-phenyl)propanedinitrile (melting point (m.p.) 145 – 147 C).

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; SYNGENTA PARTICIPATIONS AG; ZELLER, Martin; FEDOU, Nicolas; (19 pag.)WO2018/15489; (2018); 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. 14192-12-2, name is 2,5-Diiodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 2,5-Diiodobenzoic acid

EXAMPLE 1; 5-iodo-2-[[2-2[(dimethylamino)methyl]phenyl]thio]benzyl alcohol (IDAM) and (5-bromo-2-[[2-2[(dimethylamino)methyl]phenyl]thio]benzyl alcohol); The synthesis of 5-iodo-2-[[2-2[(dimethylamino)-methyl]phenyl]thio]benzyl alcohol (IDAM) and its bromo derivative (5-bromo-2-[[2-2[(dimethylamino)methyl]phenyl]thio]benzyl alcohol) was achieved by a reaction sequence outlined in Scheme 1 shown on page 37 of this application. The direct coupling of 2,5-dibromobenzoic acid (Frazer, A., J. Clin. Psychiatry. 6:9-25 (1997)) or 2,5-diiodobenzoic acid (Mathis, C. A. et al., J. Nucl. Med. 33:890(1992)) with 2-thio-N,N-dimethylbenzamide (Wong, D. T. et al. Adv. Exp. Med. & Biol., 363:77-95 (1995)) was carried out in N,N-dimethylacetamide (DMAC) with sodium methoxide to give the desired compounds in good yield (59 and 44% for 23 and 28, respectively). Only when 2-thio-N,N-dimethylbenzamide was freshly prepared, was a good coupling yield achieved. This may due to the fact that the free thiol of 22 was not stable upon prolonged standing at room temperature. The bromo compound was converted to the corresponding tri-n-butyltin derivative (Maryanoff. E. M. et al., J. Med. Chem. 33:2793-2797 (1990)) by a tetrakis(triphyenlphosphine)palladium(0)-catalyzed reaction with good yield (66%). The tin derivative was successfully converted to IDAM with excellent yield (97%), or alternatively, 2-((4-iodo-2-carboxyphenyl)thio)N,N-dimethylbenzamide (Mathis, C. A. et al., Eur. J. Pharmacol. 210:103-104 (1992)) was reduced to IDAM with 66% yield.

The synthetic route of 14192-12-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The Trustees of the University of Pennsylvania; US6921840; (2005); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 1097871-23-2, 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. 1097871-23-2, name is 1-Chloro-2,5-difluoro-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Synthesis of (S)-N-((S)-(4-Chloro-2,5-difluorophenyl)(3-fluorooxetan-3-yl)methyl)-2-methylpropane-2-sulfinamide To an oven dried, 100 mL, round bottom flask, under a nitrogen atmosphere, was added 1-chloro-2,5-difluoro-4-iodobenzene (2.41 g, 8.77 mmol) in anhydrous THF (35 mL). The resulting solution was cooled to -100 C. with an ether/liquid nitrogen bath, and then n-butyllithium (1.6M in hexanes, 5.48 mL, 8.77 mmol) was added dropwise, keeping the internal temperature between -90 and -100 C. The resulting yellow mixture was stirred between -90 and -100 C. for 30 minutes, and then (S,E)-N-((3-fluorooxetan-3-yl)methylene)-2-methylpropane-2-sulfinamide (2.0 g, 9.65 mmol) in THF (5 mL) was added dropwise via syringe, keeping the internal temperature between -90 and -100 C. The resulting mixture was stirred between -90 and -100 C. for 30 minutes and then quenched at the same temperature by dropwise addition of saturated ammonium chloride (25 mL). The mixture was diluted with water (50 mL) and ethyl acetate (50 mL). The layers were shaken and separated and the organic phase was washed with saturated aqueous sodium chloride, dried over sodium sulfate and concentrated to a viscous nearly colorless oil which was purified with silica gel using a gradient to 50% ethyl acetate/hexanes providing (S)-N-((S)-(4-chloro-2,5-difluorophenyl)(3-fluorooxetan-3-yl)methyl)-2-methylpropane-2-sulfinamide (1.64 g, 4.6 mmol) the desired single diastereomer, as a white foam. 1H NMR (400 MHz, Methanol-d4) delta 7.58-7.37 (m, 2H), 5.28 (d, J=26.1 Hz, 1H), 4.99-4.89 (m, 1H), 4.85-4.76 (m, 1H), 4.69-4.50 (m, 2H), 1.21 (s, 9H). LCMS-ESI (POS.) m/z: 356.10 (M+H)+.

The chemical industry reduces the impact on the environment during synthesis 1-Chloro-2,5-difluoro-4-iodobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; AMGEN INC.; CYTOKINETICS, INC.; Ashcraft, Luke; Boezio, Alessandro; Butler, John; Chandra, Aroop; Chuang, Chihyuan; Collibee, Scott E.; Debenedetto, Mikkel; DiMassa, Vincent; Graceffa, Russell; Malinowski, Justin; Moebius, David; Morgan, Bradley P.; Payette, Joshua; Romero, Antonio; St. Jean, JR., David; Vargas, Richard; Yeoman, John; Zhang, Hanmo; (146 pag.)US2019/77793; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 626-00-6, 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. 626-00-6, name is 1,3-Diiodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

[00121] Charge copper (I) iodide (FW 190.45, 0.90 grams, 4.72 mmol), 1,10-phenanthroline (FW 180.21, 0.83 grams, 4.62 mmol), cesium carbonate (FW 325.82, 19.00 grams, 58.30 mmol), 1 ,3-diiodobenzene (FW 329.90, 7.50 grams, 22.70 mmol), di(ethylene glycol) ethyl ether (FW 134.71, 14.06 grams, 104.40 mmol) and 100 milliliters of dry xylene in a 350 milliliter three necked round bottom flask. The reaction mixture was heated with stirring at reflex temperature for 20 hours under nitrogen. The resulting suspension was cooled to room temperature by adding 50 milliliters of toluene. Then the reaction mixture was filtered through celite and alumina. The low boiling (xylene and toluene) component was removed by a rotary evaporator and high boiling component di(ethylene glycol) ethyl ether by air bath oven at 180C under high vacuum for 2 hours. The residue was purified by flask chromatography on silica gel. The final dark yellow product was yielded 5.20 grams (67%). The product IR, and C NMR analysis shows the formation of aryl ether product. IR: neat (cm” FontWeight=”Bold” FontSize=”10″ ): 687, 763, 843, 995, 1058, 1 116, 1 157, 1 185, 1264, 1289, 1333, 1351, 1418, 1452, 1492, 1590, 2874. 13C NM (CDC13): 149.22, 121.87, 1 15.18, 70.84, 70.65, 69.83, 68.90, 66.5, 15.12.

The chemical industry reduces the impact on the environment during synthesis 1,3-Diiodobenzene. 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; WO2015/60984; (2015); A1;,
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 351447-07-9 as follows. SDS of cas: 351447-07-9

(Example 1 Synthesis of Compounds 1-42, 1-96, and I-51) [Show Image]Step 1 To a solution of Compound (5) (1.90 g, 7.25 mmol) in tetrahydrofuran (20mL), phenylisocyanate (1.0mL, 9.43mmol) and triethylamine (1.5 mL, 10.9 mmol) were added. The solution was then stirred at room temperature for 1 hour. The precipitated powder was filtered, and then washed with water. The resulting powder was further washed with diethyl ether to yield Compound 1-42 (1.95 g, 63%) as a white powder. 1H-NMR (DMSO-d6) delta12.13 (1H, s), 7.57 (2H, d, J = 8.4 Hz), 7.45 (1H, d, J = 8.1 Hz), 7.37 (2H, t, J = 7.5 Hz), 7.17 (1H, d, J = 8.4 Hz), 7.08 (1H, t, J = 7.2 Hz), 4.28 (2H, br s), 4.03 (2H, br s) LC/MS (Method A): 2.54 min, [M+H]+ = 382.3.

According to the analysis of related databases, 351447-07-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shionogi & Co., Ltd.; EP2341052; (2011); 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. 69518-17-8, name is 4-Iodophthalonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 4-Iodophthalonitrile

EXAMPLE 71 (1S,2R)-4′-(2-Hydroxy-1-methyl-4-pyridin-3-ylbutoxy)biphenyl-3,4-dicarbonitrile Prepared according to the method described in Example 12b) from (1S,2R)-4-(2-hydroxy-1-methyl-4-pyridin-3-ylbutoxy)benzeneboronic acid (0.197 g, Example 33), 4-iodo-1,2-dicyanobenzene (0.421 g, Can. J. Chem., 1985, 63, 3057), 2M aqueous sodium carbonate (0.50 ml) and tetrakis(triphenylphosphine)palladium (0) (0.054 g) in ethanol (3 ml). The reaction mixture was heated in a sealed vial at 90 C. for 4 hours. After cooling, the solution was concentrated under reduced pressure and the residue purified by chromatography over silica eluding with ethyl acetate. The residue was further purified by chromatography over silica gel eluding with dichloromethane:2-propanol (19:1). The residue was then further purified by reverse-phase HPLC eluding a gradient of 25-100% acetonitrile in 0.1 w/v aqueous ammonium acetate solution. The HPLC fractions were concentrated under reduced pressure, the residue dissolved in dichloromethane, filtered and concentrated under reduced pressure. The residue was triturated with ether to give the title to compound as a solid (0.060 g). m.p. 135.5-137 C. MS (APCI) 384 (M+H)+ 1H NMR (DMSO) 8.47-8.43(2H, m); 8.38(1H, dd); 8.25-8.12(2H, m); 7.79(2H, d), 7.63(1H, dt); 7.30(1H, dd); 7.06(2H, d); 5.03(1H, d); 4.41(1H, quintet); 3.63-3.5(1H, m); 2.9-2.75(1H, m); 2.75-2.6(1H, m); 1.95-1.8(1H, m); 1.75-1.55(1H, m); 1.24(3H, d).

The synthetic route of 69518-17-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AstraZeneca AB; US6300352; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 507-63-1,Some common heterocyclic compound, 507-63-1, name is Heptadecafluoro-1-iodooctane, molecular formula is C8F17I, 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.

Reactions were conducted in the same manner as in Example 1 except that the perfluoroethyl iodide was replaced with 1-iodoperfluorooctane (n-C8F17I). After cooling the reaction mixtures, the reaction products were analyzed by gas chromatography (GC). Table 1 shows the results.; TABLE 1 Copper Reaction Ethylene Reaction n-C8F17I catalyst temperature pressure time Conversion g g (wt. % *) C. MPa Min GC % Ex. 2 132 13.4 (10) 80 0.1 105 99.94 Ex. 3 130.8 2.66 (2) 80 0.1 120 99.71 Ex. 4 125.3 2.51 (2) 80 0.55 58 99.89 Ex. 5 155.2 3.11 (2) 120 0.1 56 99.97 Ex. 6 122.5 0.62 (0.5) 120 0.55 40 99.86 Comp. 133.2 0.13 ** 105 0.1-0.2 180 97.7 Ex. 1 * wt. % relative to n-C8F17I ** conducted using t-butylperoxyisopropyl monocarbonate (Perbutyl I) as a catalyst The conversion of each 1-iodoperfluorooctane of Examples 2-6 was more than 99.7%. The selectivity for the resulting ethylene adduct (adduct of one ethylene molecule) was 99.9% or greater in each case.

The synthetic route of 507-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Funakoshi, Yoshirou; Miki, Jun; US2005/250966; (2005); 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. 1427311-76-9, name is (S)-1-(4-Iodo-5-methoxy-2-nitrophenyl)-2,2-dimethylpropan-1-ol, A new synthetic method of this compound is introduced below., Recommanded Product: (S)-1-(4-Iodo-5-methoxy-2-nitrophenyl)-2,2-dimethylpropan-1-ol

Compound 38 (350 mg, 0.54 mmol) and (5)-l-(4-iodo-5-methoxy-2-nitrophenyl)-2,2- dimethyl- 1 -propanol (720 mg, 1.97 mmol) were heated at 110C for 45 min under a nitrogen atmosphere. The mixture was cooled down to room temperature, dissolved in MeOH (10 mL), and followed by addition of NH4F (400 mg, 11.1 mmol). The mixture was stirred at 50 C for 12 hours, concentrated in vacuo, dissolved in CH2CI2 (50 mL), and washed with brine (50 mL). The organic phase was dried over Na2S04, concentrated in vacuo, and the residue was purified by silica gel chromatography to yield 5-[(5)-l-(4-iodo-5-methoxy-2- nitrophenyl)-2,2-dimethyl-propyloxy]methyl-2′-deoxyuridine 61 (90 mg, 28%). 1HNMR (400 MHz, CDCl3): delta 8.34 (s, 1 H, Ph-H), 7.65 (s, 1 H, H-6), 7.12 (s, 1 H, Ph-H), 6.17 (t, 1 H, J = 6.8 Hz, Eta-Gamma), 5.18 (s, 1 H, Ph-CH), 4.59 (m, 1 H, H-3 ‘), 4.27 (d, 1 H, J = 12.0 Hz, 5-CH2a), 4.15 (d, 1 H, J = 12.0 Hz, 5-CH2b), 4.00 (m, 1 H, H-4’), 3.97 (s, 3 H, OCH3), 3.95 (m, 1 H, H-5’a), 3.82 (m, 1 H, H-5’b), 2.34 (m, 2 H, H-2), 0.84 (s, 9 H, C(CH3)3).

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; LASERGEN, INC.; STUPI, Brian, Philip; LI, Hong; WU, Weidong; HERSH, Megan, N.; HERTZOG, David; MORRIS, Sidney, E.; METZKER, Michael, L.; WO2013/40257; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com