Tag: M.W=200-300

Adding a certain compound to certain chemical reactions, such as: 128140-82-9, name is 1-(Difluoromethoxy)-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 128140-82-9, Quality Control of 1-(Difluoromethoxy)-4-iodobenzene

Step a) 1-(Difluoromethoxy)-4-(phenylethynyl)benzene Into a mixture of ethynylbenzene (1.9 g, 18.5 mmol), 1-(difluoromethoxy)-4-iodobenzene (5 g, 18.5 mmol), N,N-dimethylformamide (35 mL), and triethylamine (12.8 mL, 92.6 mmol) was introduced anhydrous argon for 5 minutes. Then, copper(I) iodide (1.85 mmol, 351 mg) and dichlorobis(triphenylphosphine)palladium(II) (1.11, 0.71 g) were added into the mixture and the new mixture was stirred at 60 C. for 3 hours. The mixture cooled to room temperature, poured into water and extracted with ethyl ether. The organic extracts were dried over MgSO4. Evaporation and purification on silica gel (ISCO) using hexanes/EtOAc (100/1) as the eluding solvent, gave 1-(difluoromethoxy)-4-(phenylethynyl)benzene as a clear oil (3.45 g, 76% yield). MS m/e M+244; 1H NMR (400 MHz, DMSO-d6) delta 7.2 (d, J=8.78 Hz, 2H), 7.28-7.45 (m, 4H), 7.5-7.55 (m, 2H), 7.6 (d, J=7.78 Hz, 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, 1-(Difluoromethoxy)-4-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; WYETH; US2009/48320; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, 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 40400-15-5, Recommanded Product: 2-(2-Iodophenyl)acetonitrile

General procedure: A tube was loaded with CuCl (50 mg, 0.50 mmol) and CsF (228 mg,1.50 mmol) and sealed with a rubber septum. Anhydrous acetonitrile (1 mL) was added and the mixture was cooled to 0 C. Diethyl [(trimethylsilyl)difluoromethyl]phosphonate (neat, 325 mg, 1.25 mmol) was added and the mixture was heated at 40C for 1 h, cooled to 0 C and stirred at this temperature for 1 h. Pd(PPh3)Cl2 (18 mg,0.025 mmol) was added followed by a solution of the corresponding iodoarene 1 (0.50 mmol) in MeCN (1 mL). The suspension was stirred for 16 h at 40C. The reaction mixture was diluted with diethyl ether(15 mL), the organic layer was washed with water (15 mL), Na2CO3 (concentrated solution, 15 mL), dried over Na2SO4, and solvents were carefully removed under vacuum. Reverse-phase chromatography (H2O/MeCN or MeOH, gradient: 9:1 to 0:1, rate: 1% MeCN or MeOH per minute) gave the product 2.

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, 2-(2-Iodophenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ivanova, Maria V.; Besset, Tatiana; Pannecoucke, Xavier; Poisson, Thomas; Synthesis; vol. 50; 4; (2018); p. 778 – 784;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 461-17-6, 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. 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a suspension of silver nitrite (9 g, 58.5 mmol) in diethyl ether (25 mL) at 0C was added a solution of 4-iodo-1, 1, 1-trifluorobutane, 15.02 (10 g, 42.0 mmol) in diethyl ether (25 mL) slowly through an addition funnel (approx. 15 min). The resulting mixture was vigorously stirred at 0C and warmed to rt. After 50 h, the solid material was filtered off through a celite pad. The resulting diethyl ether solution was concentrated in vacuo to give 15.03 as colorless oil, which was used without further purification.

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, 1,1,1-Trifluoro-4-iodobutane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SCHERING CORPORATION; WO2005/85197; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 401-81-0, 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. 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of the aryl halide (1 mmol), NH4OH (2 mmol), Cs2CO3 (1 mmol) and P4PVy-CuI (0.1 g) in CH3CN (10 mL) was stirred at reflux temperature. After reaction completion (moitored by TLC), the catalyst was recovered by filtration and solvent was evaporated. The residue was poured into a saturated NaCl solution, extracted with ethyl acetate and dried over anhydrous MgSO4. Evaporation of the solvent was followed by column chromatography on silica gel afforded the pure products.

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-3-(trifluoromethyl)benzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Albadi, Jalal; Shiran, Jafar Abbasi; Mansournezhad, Azam; Acta Chimica Slovenica; vol. 61; 4; (2014); p. 900 – 903;,
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. 6940-76-7, name is 1-Chloro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 6940-76-7

To a solution of TMEDA (4.36 mL, 28.9 mmol) in THF (30 mL) at -20 C was added n- butyllithium (12.03 mL, 28.9 mmol, 2.4 M solution in hexanes) over ten minutes. The mixture was stirred at 10 C for 30 minutes, then cooled to -78 C, and a solution of tert- butyl (6-chloropyridin-2-yl)carbamate (3 g, 13.12 mmol) in THF (15 mL) was added over a period of 5 minutes. After 40 minutes, copper(I) iodide (2.499 g, 13.12 mmol) was added, and the mixture was stirred at -10 C for 1 hour. l-Chloro-3-iodopropane (2.113 mL, 19.68 mmol) was added over a period of 1 minute, and the mixture was allowed to reach room temperature. After 2.5 hours the mixture was added to saturated aqueous sodium hydrogencarbonate and extracted three times with ethyl acetate. The combined organic layers were dried over sodium sulfate, filtered and concentrated. The residue was stirred in dichloromethane (30 mL), filtered through a glass- sintered funnel and concentrated to half volume and then applied onto a flash column (120 g silica), eluting with 2-20% ethyl acetate in heptane. The eluent coming off the column was passed through a column of potassium carbonate. This gave the desired product tert-butyl 7- chloro-3,4-dihydro-l,8-naphthyridine-l(2H)-carboxylate (2.637 g). Yield 74% ‘H NMR (400 MHz, Chloroform- d 7.32 (d, J = 7.9 Hz, 1H), 6.94 (d, J = 7.8 Hz, 1H), 3.81 – 3.69 (m, 2H), 2.73 (t, J= 6.6 Hz, 2H), 1.93 (p, J= 6.5 Hz, 2H), 1.54 (s, 9H).

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 6940-76-7.

Reference:
Patent; MORPHIC THERAPEUTICS, INC.; HARRISON, Bryce, A.; DOWLING, James, E.; GERASYUTO, Aleksey I.; BURSAVICH, Matthew, G.; TROAST, Dawn, M.; LIPPA, Blaise, S.; ROGERS, Bruce, N.; ZHONG, Cheng; QIAO, Qi; LIN, Fu-Yang; SOSA, Brian; BORTOLATO, Angrea; SVENSSON, Mats, A.; HICKEY, Eugene; DAY, Tyler; KIM, Byungchan; (163 pag.)WO2020/47207; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 58755-70-7, These common heterocyclic compound, 58755-70-7, name is 1-Iodo-4-methoxy-2-nitrobenzene, 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 solution of 4-iodo-3-nitroanisole (5g, 17.9 mmole) in 100 [ML METHANOL] was added [FECL3] (50mg, 0.3 mmole) and activated carbon (40 mg). The mixture was heated to reflux and hydrazine hydrate (1.75 [G,] 35 mmole) was added dropwise. The mixture was [REFLUXED] for an additional 8 hours and cooled to room temperature, filtered through Celite. The filtrate was concentrated and purified by column chromatography (eluting with 10% EtOAc in hexanes) to give 4.05 g product as pale yellow oil (91% [YILD). 1H NMR (300 MHZ, CDCL3) No. 7. ]47 [(1 H,] d, J = 8.7 Hz), 6.31 (1H, d, [J=] 2.8 [HZ),] 6.13 (1 H, dd, [J=] 2.8, 8.7 Hz), 3.73 (3H, s).

The synthetic route of 58755-70-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER INC.; WO2003/106462; (2003); 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. 74534-15-9, name is 1-Chloro-2-iodo-4-nitrobenzene, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

Iron (5 eq, 1.9 g) was added to a solution of 1-chloro-2-iodo-4-nitro-benzene (1eq, 1.95 g) in acetic acid (28 mL, 0.25M). The reaction was stirred at70C for 1 h then cooled to room temperature and filtered through celite. The crudereaction mixture was extracted with a solution of saturated ammonium chloride andethyl acetate, dried with magnesium sulfate, filtered and concentrated under vacuum toafford crude 4-chloro-3-iodo-aniline as a red oil, which was used in the next step withoutpurification.

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:
Article; Khojasteh, S. Cyrus; Yue, Qin; Ma, Shuguang; Castanedo, Georgette; Chen, Jacob Z.; Lyssikatos, Joseph; Mulder, Teresa; Takahashi, Ryan; Ly, Justin; Messick, Kirsten; Jia, Wei; Liu, Lichuan; Hop, Cornelis E. C. A.; Wong, Harvey; Drug Metabolism and Disposition; vol. 42; 3; (2014); p. 343 – 351;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 56404-21-8, name is 1-Iodo-2,4-dimethyl-3-nitrobenzene, 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 56404-21-8, Application In Synthesis of 1-Iodo-2,4-dimethyl-3-nitrobenzene

A three-necked flask equipped with a thermometer, a gas inlet, and a magnetic stirring bar was charged under argon with MnBr2 (320mg, 1.5mmol) in DMPU (25ml). CuCl (85mg, lmmol), ethyl 4-bromobutyrate (5.85g, 30mmol) and Et2Zn (2.7ml, 27mmol) were successively added. The reaction mixture turned dark red and was stirred for 4 h at 25 0C. After cooling to -30 0C, a solution of Cl2Pd(dppf) (0.925g, lOmmol) and 2,4-dimethyl-3-nitroiodobenzene (6.93g, 25mmol) in anhydrous THF (25ml) was slowly added. The reaction mixture was warmed to 25 C for 30 min and was then stirred at 65 C overnight and quenched with an aqueous 2N HCl solution (100ml). This mixture was extracted with CH2Cl2 three times, and the organic layer was dried over anhydrous Na2SO4. The solvent was removed under reduced pressure, and the crude residue obtained was purified by Biotage (hexane/EtOAc, 0-30%, 40min) to give 4.5g of yellow oily products (68 %). 1H-NMR delta (CDCl3, 300MHz): 7.13 (d, J=7.8Hz, IH), 7.03 (d, J=7.8Hz, IH), 4.12 (q, J=7.2Hz, 2H), 2.64 (t, J=7.8Hz, 2H), 2.34 (t, J=7.8Hz, 2H), 2.23 (s, 3H), 2.20 (s, 3H), 1.86 (m, J=7.8Hz, 2H), 1.24 (t, J=7.8Hz, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-2,4-dimethyl-3-nitrobenzene, and friends who are interested can also refer to it.

Reference:
Patent; VALEANT PHARMACEUTICALS INTERNATIONAL; WO2008/66900; (2008); 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 23399-70-4 as follows. COA of Formula: C7H6ClI

Step 2: At O0C5 a solution of 4-chloro-l-iodo-2-methylbenzene (642 mg, 2.53 mmol) in 5mL of pentane was treated with t-BuLi (1.68 mL of 1.7 M in pentane solution, 2.86 mmol) slowly, and stirred for 30 min. The resulting yellow mixture was cooled to – 60 0C, and a solution of N-methoxy-N-methyl-l-(trifluoroinethyl)cyclopropanecarboxamide (346 mg, 1.75 mmol) in 3.0 mL of THF was added via syringe. The reaction mixture was slowly warmed to RT in 1 h, then partitioned between a mixture of sat. ammonium chloride and EtOAc. The organic layer was separated, dried and concentrated. Purification of the residue on the ISCO (12 g column, 0-10% EtOAc:Hexanes) provided the title compound (384 mg, 83%) as a colorless amorphous solid. MS (ESI3 pos. ion) m/z: 263.1 (M+l).

According to the analysis of related databases, 23399-70-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AMGEN INC.; TASKER, Andrew; ZHANG, Dawei; WO2008/30466; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 460-37-7, The chemical industry reduces the impact on the environment during synthesis 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, I believe this compound will play a more active role in future production and life.

5-Ch[oro-N-(piperidin-4-y[)pyrazine-2-carboxamide trifluoroacetic acid salt[Intermediate 68] (722 mg, 3.00 mmol, 1 .0 eq), and potassium carbonate (2.07 g, 15.0 mmol, 5.0 eq) were suspended in 33 mL acetonitrile. Then, 1,1,1- trifluoro-3-iodopropane [CAS RN: 460-37-7] (1.01 g, 4.50 mmol, 1.5 eq) was added and the reaction mixture was heated to 70C for 4 h. On cooling, the reaction mixture was diluted with water and extracted withdichloromethane/isopropanol (4/1) (2x). The combined organic phases were washed with brine. Phase separation was conducted by the use of a Whatman filter. The volatile components were removed in vacuo and the crude material was purified via preparative MPLC (Biotage Isolera; 50 g SNAP cartridge:dichloromethane -> dichloromethane/ethanol 95/5) to give 900 mg (41% yield oftheory) of the title compound.UPLC-MS (Method 1): R = 0.58 mm; MS (ESI0): m/z = 337 [M+H].

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, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; BAeRFACKER, Lars; SIEMEISTER, Gerhard; HEINRICH, Tobias; PRECHTL, Stefan; STOeCKIGT, Detlef; ROTTMANN, Antje; WO2015/113927; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com