Tag: M.W=200-300

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. 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1,2-Dichloro-4-iodobenzene

[0268] To a solution of 1,2-dichloro-4-iodobenzene (1.0 g, 3.68 mmol) in ether (10 mL) at 0 C. was added iPrMgCl (2.2 mL, 2M in Et2O) dropwise and the resulting solution stirred at 0 C. for 30 minutes and room temperature 1 hour. The reaction mixture was recooled to 0 C. and cyclopropylacetonitrile (0.34 mL, 1.0 eq.) was added. The reaction mixture was stirred at 0 C., room temperature 1 hour, then quenched by the addition of 1N HCl. The resulting solution was stirred at room temperature 2 hours and extracted with CH2Cl2. The combined organics were dried over Na2SO4, filtered, and concentrated. The crude product was purified by flash chromatography using a 100% hexanes to 10% EtOAc in hexanes solution gradient as eluent (0.10 g, 21% yield). LCMS: MH+=227.

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 20555-91-3.

Reference:
Patent; Schering Corporation; US2003/232837; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 364-75-0,Some common heterocyclic compound, 364-75-0, name is 1-Fluoro-4-iodo-2-nitrobenzene, molecular formula is C6H3FINO2, 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.

Example 3-45-4 Preparation of 4-iodo-N-(1-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)ethyl)-2-nitroaniline To a stirred solution of 1-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)ethan-1-amine (1.93 g, 6.68 mmol) and potassium carbonate (3.70 g, 26.75 mmol) in acetonitrile (75 mL) was added 1-fluoro-4-iodo-2-nitrobenzene (2.14 g, 8.02 mmol). The mixture was heated to reflux. After 16 h, the orange mixture was allowed to cool to room temperature and was diluted with water (150 mL). The mixture was extracted with dichloromethane (3*75 mL), and the combined organic phases were dried over magnesium sulfate, filtered, and concentrated to provide 3.82 g of an orange solid. Trituration of the crude material with hexanes afforded 3.17 g (89%) of 4-iodo-N-(1-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)ethyl)-2-nitroaniline as a bright orange solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Fluoro-4-iodo-2-nitrobenzene, its application will become more common.

Reference:
Patent; KANE, JR., John L.; MATTHEWS, Gloria; METZ, Markus; KOTHE, Michael; LIU, Jinyu; SCHOLTE, Andrew; US2015/158847; (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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, A new synthetic method of this compound is introduced below., Safety of 1,3-Dichloro-5-iodobenzene

To a mixture of (1R, 3r, 5S) -tert-butyl 3-hydroxy-8-azabicyclo [3.2.1] octane-8-carboxylate (5.00 g, 22.00 mmol) in toluene (50 mL) was added 3, 5-dichloroiodobenzene (6.00 g, 22.00 mmol) , cesium carbonate (21.50 g, 66.00 mmol) , copper (I) iodide (0.63 g, 3.30 mmol) , 3, 4, 7, 8-tetramethyl-1, 10-phenantroline (1.60 g, 6.60 mmol) and molecular sieves (4A, 5.00 g) . The reaction mixture was degassed by passing a stream of argon through it and then heated at 80 in a sealed vial for 120 hours. After cooling to ambient temperature, the reaction mixture was diluted with ethyl acetate (150 mL) and filtered over diatomaceous earth. Concentration of the filtrate in vacuo gave a residue which was purified by flash chromatography (0 to 20ethyl acetate in hexanes) to afford the title compound as a yellowish oil (3.80 g, 46) :1H NMR (300 MHz, CDCl3) delta 6.93-6.90 (m, 1H) , 6.71-6.69 (m, 2H) , 4.59-4.53 (m, 1H) , 4.28-4.09 (m, 2H) , 2.24-1.85 (m, 8H) , 1.45 (s, 9H) MS (ES+) m/z 316.1, 318.1 (M -55) .

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GENENTECH, INC.; XENON PHARMACEUTICALS INC.; ANDREZ, Jean-Christophe; BICHLER, Paul Robert; CHEN, Chien-An; CHOWDHURY, Sultan; DECKER, Shannon Marie; DEHNHARDT, Christoph Martin; FOCKEN, Thilo; GRIMWOOD, Michael Edward; HEMEON, Ivan William; JIA, Qi; LI, Jun; LIU, Zhiguo; ORTWINE, Daniel F.; SAFINA, Brian; SUTHERLIN, Daniel; SHENG, Tao; SUN, Shaoyi; WHITE, Andrew D.; WILSON, Michael Scott; ZENOVA, Alla Yurevna; ZHU, Jiuxiang; WO2015/78374; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, 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. Safety of 1-Iodo-4-(trifluoromethoxy)benzene

To a solution of l-iodo-4-(trifIuoromethoxy)benzene (1.087 mL, 6.94 mMol) and TMS- acetylene (1.166 ml, 8.33 mmol) in THF (30ml) were added Copper(I) iodide (0.066 g, 0.347 mMol), Trans-Bis(triphenylphosphine)palladium(II)chloride (0.244 g, 0.347 mmol) and triethylamine (2.90 ml, 20.83 mmol). After stirring for 3h at room temperature, the reaction mixture was concentrated. The residue was dissolved in heptane, filtered through a plug of silica gel and concentrated to give the desired product as oil. Mass Spectra (m/e): 259 (M+H)

The synthetic route of 1-Iodo-4-(trifluoromethoxy)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK & CO., INC.; WO2008/133867; (2008); 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. 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., Application In Synthesis of 4-Chloro-2-iodobenzoic acid

To a solution of 4-chloro-2-iodobenzoic acid (1-1, X?I) (CAS :13421-13-1; Aldrich, SKU: 560146) (3 g, 10.62 mmol) and N,O-dimethylhydroxylamine hydrochloride (CAS : 6638-79-5; Sigma Aldrich, SKU: D163708) (1.2 g, 12.31 mmol) in dimethylformamide (DMF) (30 mL), was added dropwise triethyl amine (TEA) (7.4 mL, 53.14 mmol), followed by the addition of (1-[bis(dimethylamino)methylene]-1H-1,2,3-triazolo[4,5-b]pyridinium 3-oxid hexafluorophosphate) (HATU) (6.1 g, 16.05 mmol). The reaction mixture was stirred at RT for 16 h and then diluted with CH2Cl2 and H2O, and the aqueous layer was extracted with CH2Cl2 (4×20 mL). The combined organic layers were washed with brine, dried over Na2SO4, filtered, concentrated in vacuo and purified by silica gel chromatography (ethyl acetate/hexanes 1:4) to afford the title compound as a white solid (3.2 g. LCMS (MH+): 325.9. 1H NMR (400 MHz, CDCl3-d): delta 3.11-3.38 (m, 3H), 3.47-3.90 (m, 3H), 7.20 (d, J=8 Hz,1H), 7.37 (d, J=2 Hz, 1H), 7.84 (s,1H).

The synthetic route of 13421-13-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Karos Pharmaceuticals, Inc.; De Lombaert, Stephane; Goldberg, Daniel R.; (12 pag.)US2016/257633; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 6828-35-9, 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. 6828-35-9, name is 5-Chloro-2-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

5-Chloro-2-(phenylethynyl)aniline To 5-chloro-2-iodoaniline (1.27 g, 5.0 mmol) and ethynylbenzene (0.60 ml, 5.5 mmol) in Et3N (10 ml) was added CuI (5.0 mg, 0.025 mmol) and Pd(PPh3)2Cl2 (18 mg, 0.025 mmol) and the mixture was stirred at room temperature for 16 hours, diluted with EtOAc and was filtered through a pad of Celite. The filtrate was concentrated and the residue was purified by flash column chromatography on silica gel (0-10% EtOAc in hexanes) to yield Intermediate 14 as beige solid (1.12 g, 98%). 1H NMR (CHLOROFORM-d) delta: 7.46-7.56 (m, 2H), 7.32-7.39 (m, 3H), 7.28 (d, J=8.2 Hz, 1H), 6.66-6.75 (m, 2H), 4.37 (br. s., 2H).

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, 5-Chloro-2-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ALLERGAN, INC.; YUAN, HAIQING; BEARD, RICHARD L.; LIU, XIAOXIA; DONELLO, JOHN E.; VISWANATH, VEENA; GARST, MICHAEL E.; US2013/231338; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, 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: 1-Chloro-3-iodopropane

To a 2-L round-bottom flask was added methyl 4-hydroxy-3-methoxybenzoate (100 g, 548.93 mmol, 1.00 eq.), 1-chloro-3-iodopropane (224 g, 1.10 mol, 2.0 eq.), K2C03 (22.7 g, 3.00 eq.) followed by MeCN (1 L). The resulting mixture was allowed to stir at 80 C for 3 h. The mixture wascooled to rt, the solids were filtered and washed with EtOAc. The filtrate was concentrated under reduced pressure to afford methyl 4-(3-chloropropoxy)-3-methoxybenzoate as a white solid (12890%).

The synthetic route of 1-Chloro-3-iodopropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLOBAL BLOOD THERAPEUTICS, INC.; YU, Ming; LI, Zhe; XU, Qing; YEE, Calvin; SETTI, Lina; SHAM, Hing; (188 pag.)WO2019/36384; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 117832-17-4, 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 117832-17-4 as follows.

General experimental procedure: o-iodoaniline (1.0 mmol) and phenyl isothiocyanate (1.2 mmol) was mixtured and stirred for 1 h at room temperature (Method A), or o-iodoaniline (1.0 mmol) and phenyl isothiocyanate (1.2 equiv) was mixtured and stirred for 1 h at melting point temperature of phenyl isothiocyanate (Method B), or o-halobenzothioureas (1.0 mmol) (Method C), then anhydrous DMSO (5 ml) and base (3.0 mmol) was added, the stirring continued for about 5-10 h at 130 C (TLC monitor). After the reaction was completed, the reaction mixture was cooled to room temperature and ice-water was added, then the mixture was extracted with EtOAc. The combined organic phase was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under vacuum and then the residue was purified by column chromatography (eluent: petroleum ether/ethyl acetate (5:1 to 7:1)) on silica gel to provide the desired product.

According to the analysis of related databases, 117832-17-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Wang, Rui; Chen, Zhi; Yue, Liang; Pan, Wei; Zhao, Jun-Jie; Tetrahedron Letters; vol. 53; 34; (2012); p. 4529 – 4531;,
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. 2265-91-0, name is 1,3-Difluoro-5-iodobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,3-Difluoro-5-iodobenzene

Example 1.93: Preparation of 2-(((lr,4r)-4-((3-(3,5-Difluorophenyl)-3- phenylureido)methyl)cyclohexyl)methoxy)acetic Acid (Compound 44).; Step A: Preparation of 3,5-Difluoro-iV-phenylaniline.; In a 5 mL microwave reaction vial was placed aniline (0.298 g. 3.20 mmol) and 1,3- difluoro-5-iodobenzene (0.768 g, 3.20 mmol) in toluene (3 mL). KOH (0.323 g, 5.76 mmol) in water (650 muL) and N,N,N-trimethylhexadecan-l-ammium bromide (6.30 mg, 0.017 mmol) were added to the vial with stirring. After the reaction was warmed to 90 0C, bis[tri(f- butylphosphine]palladium[0] (0.016 g, 0.032 mmol) was added and the reaction was stirred at 150 0C for 4 h and then 160 0C for 2 h. The mixture was diluted with water and brine, and extracted with toluene. The toluene extract was subsequently washed with water, dried over MgSO4 and concentrated. The residue was purified by flash column chromatography to provide the title compound as a brown oil (0.132 g). LCMS m/z = 206.2 [M+H]+; 1H nuMR (400 MHz, DMSO-J6) delta ppm 6.54 (tt, J= 9.35, 2.27 Hz, IH), 6.63 (dd, J= 10.48, 2.15 Hz, 2H), 7.01 (dt, 7 = 14.65, 1.14 Hz, IH), 7.17 (dd, J= 8.59, 1.01 Hz, 2H), 7.34 (t, J= 7.83 Hz, 2H), 8.69 (s, IH).

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; ARENA PHARMACEUTICALS, INC.; WO2009/117095; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 13421-00-6, 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. 13421-00-6, name is 5-Chloro-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

C. The starting 2-chloro-11H-dibenz(b,f)-1,4-oxathiepin is a novel compound which may be prepared by the following procedure: A solution of 120 g of 5-chloro-2- iodobenzoic acid (K. Pelz et al., Collect.Czech.Chem.Commun. 33, 1852, 1968) in 145 ml of tetrahydrofuran is stirred and treated at 10-20 C. for 45 minutes with 16.1 g of sodium borohydride. The mixture is then stirred for 30 minutes at this temperature and treated with a solution of 80.3 g (71.4 ml) of boron trifluoride etherate in 40 ml of tetrahydrofuran. It is stirred for another 3 hours and while cooling with ice-cold water it is decomposed at a maximum temperature of 8 C. with 50 ml of 5% hydrochloric acid added dropwise. It is diluted with water and extracted with benzene. The extract is washed with a 5% sodium hydroxide solution and water, dried with magnesium sulfate and evaporated. There are obtained 100 g (96%) of crude 5-chloro-2-iodobenzyl alcohol with m.p. of 115-117 C. The analytically pure substance is obtained by crystallization from ethanol; m.p. 116-117 C.

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, 5-Chloro-2-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SPOFA, spojene podniky pro zdravotnickou vyrobu; US4431808; (1984); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com