Iodides-buliding-blocks

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 77317-55-6 as follows. Formula: C8H8INO2

To a round bottom flask was added methyl 2-amino-5-iodobenzoate (5.00 g, 18.1 mmol) and di-tert-butyl dicarbonate (3.94 g, 18.1 mmol). The flask was sealed and evacuated/backfilled with nitrogen (3x) . Tetrahydrofuran (90 ml_) was added, and the reaction mixture was heated to 60 C overnight. 4-Dimethylaminopyridine (1.10 g, 9.02 mmol) was added, and the reaction mixture was heated for 1.5 hours. The reaction mixture was cooled to room temperature. Ethyl acetate and water were added, and the layers were separated . The organic layers were combined, dried over anhydrous sodium sulfate, filtered, and concentrated. Purification by flash column chromatography using ethyl acetate/hexanes as eluent provided the title compound as a pale yellow solid ( 1.70 g, 20%) : *H NMR (400 MHz, CDCI3) delta 8.32 (d, J = 2.1 Hz, 1H), 7.84 (dd, J = 8.3, 2.2 Hz, 1H), 6.93 (d, J = 8.3 Hz, 1H), 3.87 (s, 3H), 1.38 (s, 18H) ; EIMS m/z 478 ([M + H]+) .

According to the analysis of related databases, 77317-55-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DOW AGROSCIENCES LLC; GIAMPIETRO, Natalie C.; CROUSE, Gary D.; SPARKS, Thomas C.; DEMETER, David A.; (242 pag.)WO2017/40742; (2017); 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. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H4F13I

Specifically, first, 20.00 g (42.19 mmol) of 2- (perfluorohexyl) ethyl iodide and 5.32 g (42.19 mmol) of 4-mercaptophenol were placed in a 250 mL round bottom flask,Was dissolved in 100 mL of acetone, and 5.83 g (42.19 mmol) of potassium carbonate was added thereto, and the mixture was refluxed at 70 C. for 24 hours. Disappearance of the raw material was confirmed by HPLC, and cyclopentyl methyl ether, water and 1 N hydrochloric acid were added thereto. The aqueous layer was removed and the remaining organic layer was washed with water and saturated brine. After washing, the organic layer was allowed to stand for 1 hour by using anhydrous magnesium sulfate and dried, then the magnesium sulfate was removed using a fold filtration, and the obtained solution was concentrated under reduced pressure. The residue obtained by concentration was purified by column chromatography (packing agent: silica gel, developing solvent: chloroform, the same shall apply hereinafter) to obtain 19.13 g (40.51 mmol) of compound (B) as a colorless solid. The melting point of the obtained compound (B) (measured by a trace amount melting point measuring apparatus “Yanaco Micro Melting Point Apparatus MP-J3”, the same applies hereinafter) was 68 to 70 C., and the yield was 96%. Further, an infrared spectrophotometer (trade name “IRPrestige-21” manufactured by Shimadzu Corporation)Similarly. “JEOL JMN-LA 500” manufactured by Nippon Denshi Co., Ltd. When the solvent is CDCl 3, the internal standard is tetramethylsilane, and when the solvent is DMSO-d 6, the internal standard is DMSO-H 2.49 ppm, the same shall apply hereinafter), the compound (B) was identified.

The synthetic route of 2043-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Yamaguchi University; Okamoto, Hiroaki; Morita, Yuki; (74 pag.)JP2016/175873; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 20555-91-3, name is 1,2-Dichloro-4-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 20555-91-3, HPLC of Formula: C6H3Cl2I

Step 3: l-(3, 4-Dichlorophenyl)-4-phenyl-4-[(2-propenyloxy)methyl]imidazolidine-2, 5-dione; [00327] 0.7 g of 4-phenyl-2-(propenyloxy)imidazolidine-2,5-dioneare dissolved in 2 mL DMAC and780 mg of l,2-dichloro-4-iodo-benzene are added, followed by 234mg of copper (I) oxide. The mixture is warmed at 1600C for 3 hours. At rt the mixture is diluted with a 20% aqueous solution of ammonia and extracted with ethyl acetate. The organic layer is dried over sodium sulfate, filtered and evaporated. The crude product is purified by chromatography over silica gel while eluting with the 2/1 heptane/ethyl acetate mixture. delta 1H NMR (DMSO): 3.70 (d, IH); 4.08 (m, 2H); 4.15 (d, IH); 5.17 (d, IH); 5.25 (d, IH); 5.88 (ddt, IH); 7.38-7.50 (m, 4H); 7.62 (d, 2H); 7.67 (m, IH); 7.78 (d, IH), 9.40(s, IH).LCMS: (Rt = 3.44 min): no ionization

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; GALAPAGOS NV; NIQUE, Francois; JAGERSCHMIDT, Catherine; BLANQUE, Roland; LEFRANCOIS, Jean-Michel; PEIXOTO, Christophe; DEPREZ, Pierre; TRIBALLEAU, Nicolas; WIGERINCK, Piet, Tom, Bert, Paul; NAMOUR, Florence, Sylvie; WO2010/29119; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 160938-18-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 160938-18-1 name is 4-Chloro-2-iodo-1-nitrobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Under an argon atmosphere, to a 500 ml, three neck flask, 20.00 g (170.7 mmol) of indole, 7.67 g (0.1 equiv, 34.1 mmol) of Pd(OAc)2, 94.38 g (2 equiv, 682.9 mmol) of K2CO3, 58.07 g (1.2 equiv, 204.9 mmol) of 4-chloro-2-iodo-1-nitrobenzene and 341 ml of 1,4-dioxane were added in that order, followed by heating, stirring and refluxing for about 24 hours. After cooling to room temperature, the reaction product was filtered with celite to separate insoluble residue, water was added to the remaining reaction product, and an organic layer was separately taken. To an aqueous layer, toluene was added, and an organic layer was extracted once more. The organic layer thus collected was washed with a saline solution and dried with MgSO4. MgSO4 was separated, and the organic layer was concentrated, and then, the crude product thus obtained was separated by silica gel column chromatography (using a mixture solvent of hexane and toluene as a developer) to obtain Intermediate IM-9 (20.95 g, yield 45%) as a white solid compound. A molecular ion peak of m/z=272 was observed by measuring FAB-MS, and from the result, the product was identified as Intermediate IM-9.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-2-iodo-1-nitrobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Samsung Display Co., Ltd.; UNO, Takuya; (126 pag.)US2019/372019; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 2401-21-0,Some common heterocyclic compound, 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, molecular formula is C6H3Cl2I, 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.

PREPARATION 5 A mixture of p-aminopropiophenone (5 g), pyridine (2.7 g), and iodobenzene dichloride (7.5 g) in tetrahydrofuran (150 ml) was stirred for 3 hours at 0¡ã to 5¡ã C. The insoluble materials were filtered, and the filtrate was concentrated under reduced pressure. The residue was dissolved in chloroform, washed with an aqueous solution of sodium hydrogen sulfite, dried over magnesium sulfate, and concentrated to give an oil (8.8 g). The oil was subjected to column chromatography on silica gel eluding with chloroform. The fractions containing the desired compound were combined and concentrated under reduced pressure. The residual oil was triturated with a mixture of hexane and ethyl acetate to give pale yellow crystals of 4′-amino-3′-chloropropiophenone (1.1 g). mp: 79¡ã to 80¡ã C. IR (Nujol): 3500, 3380, 1670, 1620, 1595 cm-1. NMR (CDCl3, delta): 1.20 (3H, t, J=7 Hz), 2.88 (2H, q, J=7 Hz), 4.50 (2H, broad s), 6.72 (1H, d, J=8 Hz), 7.68 (1H, dd, J=8 Hz, 2 Hz), 7.88 (1H, d, J=2 Hz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,2-Dichloro-3-iodobenzene, its application will become more common.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US4866091; (1989); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 181765-86-6, These common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, 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.

Methyl 5-bromo-2-iodobenzoic acid (25.0 g, 73 mmol) was charged in a 500 mL round bottom flask reactor,4-dibenzofuran boronic acid (18.7 g, 88 mmol), tetrakis (triphenylphosphine) palladium (1.7 g, 0.15 mmol), potassium carbonate (20.2 g, 146.7 mmol)And 125 mL of toluene, 125 mL of tetrahydrofuran, 50 mL of water. The temperature of the reactor was raised to 80 C and stirred for 10 hours.After completion of the reaction, the temperature of the reactor was lowered to room temperature, and the organic layer was extracted with ethyl acetate and separated.The organic layer was concentrated under reduced pressure and then separated by column chromatography to obtain (75.0 g, 60.1%).

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC Co., Ltd.; Che Chunxu; Po Xipei; Po Shangyu; Shen Youna; Jin Xida; (130 pag.)CN107207454; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, 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: 1,1,1-Trifluoro-3-iodopropane

Example 296A 3-(2-Methoxyethyl)-5-methyl-2,4-dioxo-1-(3,3,3-trifluoropropyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carbaldehyde 341 mg (2.47 mmol) of potassium carbonate were added to a solution of 285 mg (0.98 mmol) of the compound from Ex. 53A in 9 ml of DMF, and the mixture was stirred at RT for 15 min. Then 664 mg (2.96 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred at 50 C. for 19 h. The DMF was then very substantially distilled off and the remaining residue was partitioned between semisaturated sodium chloride solution (200 ml) and ethyl acetate (100 ml). The aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The residue obtained was chromatographed using a silica gel cartridge (Biotage, 50 g of silica gel, eluent: hexane/ethyl acetate). 254 mg (69% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.11 (s, 1H), 4.18 (t, 2H), 4.06 (t, 2H), 3.53-3.48 (m, 2H), 3.24 (s, 3H), 2.84-2.75 (m, 5H). LC/MS (Method 3, ESIpos): Rt=1.10 min, m/z=365 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 460-37-7, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, 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. Product Details of 460-37-7

1,2-Dibromoethane (0.04 ml, 0.51 mmol) was added to a stirred suspension of zinc (0.45 g, 6.82 mmol) in DMF (3.5 ml). The mixture was stirred at 90 C for 30 min. under nitrogen and then chlorotrimethylsilane (0.013 ml, 0.102 mmol) was added. The mixture was stirred at RT for a further 30 min. and then a solution of 3-iodo-l,l,l- trifluoropropane in DMF (2 ml) was added dropwise . The mixture was stirred at 45 C for 2.5 h. and the resulting solution was transferred via syringe to a second flask charged with intermediate 34 (0.144 g, 0.34 mmol) andbis(triphenylphosphine)palladium (II) dichloride (0.024 g, 0.034 mmol) under nitrogen. The mixture was stirred at 40 C for 1 h. and then allowed to cool down to RT. A saturated solution of ammonium chloride was added and the mixture was extracted with EtOAc. The organic layer was separated, washed with a saturated solution of ammonium chloride and brine, dried (Na2S04), filtered and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica; EtOAc in heptane 0/100 to 100/0). The desired fractions were collected and evaporated in vacuo to yield intermediate 38 (0.07 g, 52%) as a pale brown solid.

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BARTOLOME-NEBREDA, Jose, Manuel; CONDE-CEIDE, Susana; MACDONALD, Gregor, James; PASTOR-FERNANDEZ, Joaquin; VAN GOOL, Michiel, Luc, Maria; MARTIN-MARTIN, Maria, Luz; VANHOOF, Greta, Constantia, Peter; WO2011/110545; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, molecular formula is C8H6IN, 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. Quality Control of 2-(2-Iodophenyl)acetonitrile

A mixture of 4-((benzyloxy)methyl)-2H-1,2,3-triazole I58 (1.7 g, 9.0 mmol), 2-(2- iodophenyl)acetonitrile (3.0 g, 12.0 mmol), Fe(acac)3 (1.1 g, 3.0 mmol), CuO (720 mg, 0.9 mmol) and Cs2C03 (6.0 g, 18.0 mmol) in DMF (60 mL) was heated at 90 C under N2 for 30 h. The mixture was diluted with water and extracted with EtOAc. The combined organic extracts were washed with brine, dried over anhydrous Na2S04, filtered and concentrated under reduced pressure to give the title compound (1.4 g, 51 %) as a yellow oil. LCMS-D: Rt 2.87 min; m/z 305.1 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 40400-15-5, its application will become more common.

Reference:
Patent; CTXT PTY LIMITED; MORROW, Benjamin Joseph; FOITZIK, Richard Charles; CAMERINO, Michelle Ang; LAGIAKOS, Helen Rachel; WALKER, Scott Raymond; BOZIKIS, Ylva Elisabet Bergman; STEVENSON, Graeme Irvine; CUZZUPE, Anthony Nicholas; STUPPLE, Paul Anthony; (313 pag.)WO2019/43139; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 51628-12-7, 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. 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 26 Preparation of 2-{4-[4-(1-Methyl-2-{[(methylethyl)sulfonyl]amino}ethoxy)phenyl]phenyl}ethanenitrile. Preparation of 4-(cyanomethyl-phenylboronic acid, pinacol ester. Using the method of Murata, M., et al., Y. J. Org. Chem, 62 6458-6459 (1997), 4-iodophenylacetonitrile (23.9 g, 0.100 mol), Et3N (42 ML, 0.30 mol), acetonitrile (400 ML) and Pd(dppf)2Cl2 catalyst ([1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex with CH2Cl2) were combined in a 1 L flask and the resulting solution was evacuated and purged with nitrogen three times.The pinacolborane (22 ML, 0.15 mol) was added and the mixture was heated at reflux for 3 h. 1H NMR analysis of an aliquot indicated complete consumption of starting 4-iodophenylacetonitrile.The mixture was cooled to room temperature, concentrated to an oil and taken up in CH2Cl2.This solution was extracted with 0.1 N HCl (3*100 ML) and the organic phase was separated, concentrated and re-dissolved in methyl tert-butyl ether (MTBE).The MTBE solution was passed through a filter packed with silica gel (300 g).The eluant was concentrated to a dark red oil.This oil was extracted with hexanes (500 ML) and the soluble fraction was decanted away from a black oil (5 g). MTBE (5 ML) was added to this oil to give a suspension that was filtered through Celite.This filtrated was combined with the hexanes fraction and the solution was concentrated to an oil.Finally, the oil was re-dissolved in di-isopropyl ether (150 ML) and was diluted with hexanes (400 ML).This mixture was allowed to stand for 2 h, and then filtered to remove a dark precipitate.The resulting amber filtrate was concentrated to an oil, re-dissolved in hexanes (400 ML) and concentrated to 75 ML without added heat.This treatment resulted in the precipitation of the desired intermediate title compound as a golden waxy solid that was air-dried to afford 23.0 g (96.2%): 1H NMR (CDCl3, 300 MHz): delta7.8 (d, 2H); 7.35 (d, 2H); 3.8 (s, 2 H) 1.15 (s, 12H).

The synthetic route of 2-(4-Iodophenyl)acetonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Davison, Joshua Zwick; Jones, Winton Dennis; Zarrinmayeh, Hamideh; Zimmerman, Dennis Michael; US2003/225266; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com