Month: April 2021

Related Products of 42861-71-2, 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 42861-71-2 as follows.

Step 1 : 3-(2- {4-[4-(2-Trifluoromethylbenzoyl)piperazino]phenyl-l-ethynyl)phenyl acetate: Prepared by coupling reaction of Intermediate 2 with 3-iodophenyl acetate to give the product as an off-white solid; IR (KBr) 2923, 2207, 1767, 1638, 1507, 1201, 1010, 775 cm”1; 1H NMR (300 MHz, DMSO-J6) delta 2.27 (s, 3H), 3.17-3.28 (m, 2H), 3.41-3.80 (m, 6H), 6.99 (d, J = 8.7 Hz, IH), 7.15 (d, J = 7.8 Hz, IH), 7.30 (s, IH), 7.38-7.47 (m, 2H), 7.55 (d, J= 7.5 Hz, IH), 7.68-7.80 (m, 3H), 7.85 (d, J = 7.8 Hz, IH), 8.32 (d, J = 1.8 Hz, IH); ESI-MS (m/z) 494.53 (M+H)+.

According to the analysis of related databases, 42861-71-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; WO2008/62276; (2008); A2;,
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. 98-61-3, name is 4-Iodobenzenesulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

General procedure: A 10 ml dried round bottom flask was charged sequentially with a stirring bar, Pd(PhCN)2Cl2 (0.02 mmol, 10 mol %), K2CO3 (05 equiv), p-toluene sulfonyl chloride (1.5 equiv) and 4 ? molecular sieve (50 mg). Dry dioxane (1 ml) and alpha-methyl vinyl pyridine (0.2 mmol, 1 equiv) were added into the mixture in sequence, and the resultant mixture was stirred at 120 C under 1 atm of oxygen (balloon pressure) for 24 h. After cooling down, the mixture was diluted with ethyl acetate and filtered via Celite. After removing the organic solvent under reduced pressure, the crudeproduct was purified by silica gel flash column chromatography (EtOAc/hexane mixtures). And 3a was obtained in 71% yield as a white solid. Mp=98-99 C; Rf=0.35 (EA/Hexane=3:7). 1H NMR (300 MHz, CDCl3) delta 8.58 (d, J=4.23 Hz, 1H), 7.87 (d, J=8.25 Hz, 2H), 7.68-7.74 (td, J=7.77, 1.70 Hz, 1H), 7.50 (d, J=7.95 Hz, 1H), 7.34 (d, J=8.25 Hz, 2H), 7.25-7.29 (m, 2H), 2.59 (s, 3H), 2.43 (s, 3H); 13C NMR (75 MHz, CDCl3) delta 155.8, 149.6, 149.3, 144.2, 139.0, 136.8, 129.9, 127.4, 124.1, 121.0, 21.5, 15.0; IR (film, cm-1): 3020, 1597, 1581, 1568, 1465, 1431, 1311, 1301, 1215, 1145, 1085; HRMS m/z calculated for C14H13O2 [M+H]+: 213.2887; found 213.2882.

According to the analysis of related databases, 98-61-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Xu, Yun-He; Wang, Min; Lu, Ping; Loh, Teck-Peng; Tetrahedron; vol. 69; 22; (2013); p. 4403 – 4407;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, 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. category: iodides-buliding-blocks

Oxalylchloride (176 kg; 1386 mol; 1.14 eq) is added to a mixture of 2-chloro-5-iodo benzoic acid (343 kg; 1214 mol) (compound IX.1), fluorobenzene (858 kg) and N,N-dimethylformamide (2 kg) within 3 hours at a temperature in the range from about 25 to 30 C. (gas formation). After completion of the addition, the reaction mixture is stirred for additional 2 hours at a temperature of about 25 to 30 C. The solvent (291 kg) is distilled off at a temperature between 40 and 45 C. (p=200 mbar). Then the reaction solution (911 kg) is added to aluminiumchloride AlCl3 (181 kg) and fluorobenzene (192 kg) at a temperature between about 25 and 30 C. within 2 hours. The reaction solution is stirred at the same temperature for about an additional hour. Then the reaction mixture is added to an amount of 570 kg of water within about 2 hours at a temperature between about 20 and 30 C. and stirred for an additional hour. After phase separation the organic phase (1200 kg) is separated into two halves (600 kg each). From the first half of the organic phase solvent (172 kg) is distilled off at a temperature of about 40 to 50 C. (p=200 mbar). Then 2-propanole (640 kg) is added. The solution is heated to about 50 C. and then filtered through a charcoal cartouche (clear filtration). The cartouche may be exchanged during filtration and washed with a fluorobenzene/2-propanole mixture (1:4; 40 kg) after filtration. Solvent (721 kg) is distilled off at a temperature of about 40 to 50 C. and p=200 mbar. Then 2-propanole (240 kg) is added at a temperature in the range between about 40 to 50 C. If the content of fluorobenzene is greater than 1% as determined via GC, another 140 kg of solvent are distilled off and 2-propanole (140 kg) is added. Then the solution is cooled from about 50 C. to 40 C. within one hour and seeding crystals (50 g) are added. The solution is further cooled from about 40 C. to 20 C. within 2 hours. Water (450 kg) is added at about 20 C. within 1 hour and the suspension is stirred at about 20 C. for an additional hour before the suspension is filtered. The filter cake is washed with 2-propanole/water (1:1; 800 kg). The product is dried until a water level of <0.06% w/w is obtained. The second half of the organic phase is processed identically. A total of 410 kg (94% yield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. The synthetic route of 2-Chloro-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings. Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2011/237789; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, 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. SDS of cas: 19094-56-5

[0238] A 250 mL of 4-necked flask equipped with thermometer and mechanical stirring was charged with NaBH4 (4.16 g, 0.11 mol) and THF (60 mL) under argon. After cooling to 0-5 C with stirring, a solution of iodine in THF (12.7 g I2 in 25 mL THF) was added slowly dropwise over 30 min and the reaction temperature was maintained below 10 C. After the addition was completed, a solution of 2-chloro-5-iodobenzoic acid (15.0 g, 50 mmol) in THF (20 mL) was added dropwise over 30 min and kept the reaction temperature below 10 C. After stirring for another 3 h at 20-25 C, the reaction mixture was heated to reflux for additional 16 h and monitored by TLC (PE/E A = 1 : 1, Rf = 0.2). The mixture was cooled to 20-25 C and poured into ice water (100 mL), extracted with ethyl acetate (2 x 100 mL), washed with water (2 x 100 mL), brine (100 mL), concentrated and the residue was purified by flash chromatography (PE:EA = 20: 1 as eluant, 200 mL) to give an off-white solid. Yield: 10.0 g (70%) MS ESI (m/z): 269 [M+l]+.

The synthetic route of 2-Chloro-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THERACOS, INC.; XU, Baihua; LV, Binhua; XU, Ge; SEED, Brian; ROBERGE, Jacques; WO2013/152476; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 335349-57-0, name is 5-Chloro-4-iodo-2-nitroaniline, molecular formula is C6H4ClIN2O2, 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. Computed Properties of C6H4ClIN2O2

Compound 2S 2-nitro-4-iodo-5-chloroaniline (2200 g, 7.4 mol) was added to a solution of 7.3 L of dimethylsulfoxide (DMS0) and7.3 L methanol (Mu0H) mixed solution, then add K0H (1040g, 18.4mo 1),Temperature control at 30 C plus finish. And then heated to 60 C reaction 4h, TLC detection reaction is complete, then cooled to room temperature, the reaction solution into 10L of water, Stirred for 15min, filtered, the filter cake washed with water to neutral, drying the compound 3S 3-methoxy-4-iodo-5-nitro-aniline(2100 g, 7.14 mol) Yield 97%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 335349-57-0, its application will become more common.

Reference:
Patent; Shanghai Bide Pharmaceutical Technology Co., Ltd.; Mi Taoran; Huang Liangfu; Lu Qinjie; Zhang Ruihao; Li Xinling; (6 pag.)CN106496037; (2017); A;,
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 39998-81-7 as follows. name: 2-Fluoro-4-iodo-1-methylbenzene

Example 7: (Compound N7)2-Amino-l-ethyl-7-((R)-3-hydroxy-4-methoxy-3-methyl-but-l-ynyl)-3- (lH-imidazol-2-yl)-lH-quinolin-4-one7.1: 2-Fluoro-4-iodo-benzoic acid13.39 g (84.74 mmol) potassium permanganate were added to a suspension of 5 g (21.18 mmol) of 2-fluoro-4-iodo-toluene and 25.13 g (317.77 mmol) of pyridin in water. The mixture was heated and stirred at 70C during 18 hours. As the reaction was not finished, 3.34 g (21.18 mmol) of potassium permanganate were added to the reaction mixture at room temperature and the mixture was stirred for another 6 hours at 70C. The reaction mixture was then filtered through a celite pad, which was then washed with water and ethyl acetate. After decantation, the aqueous phase was acidified to pH =1 with an aqueous solution of HC1 6N. A white solid was first filtered and the aqueous phase extracted three times with ethyl acetate. The combined organic phases were dried over MgS04 and the solvents were evaporated off under reduced pressure. The filtered white solid and the solid extracted with ethyl acetate were combined to give 4.1 g.Yield = 73%.MH+ = 266.9 (C7H4FI02). 1H NMR (DMSO-d6, 400MHz): delta 13.49 (broad signal, 1H); 7.88 (d, 1H); 7.78 (d, 1H); 7.65 (d, 1H).

According to the analysis of related databases, 39998-81-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SANOFI; BRAUN, Alain; DUCLOS, Olivier; LASSALLE, Gilbert; LORGE, Franz; MARTIN, Valerie; RITZELER, Olaf; STRUB, Aurelie; WO2012/159959; (2012); 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. 3930-83-4, name is 2-Iodobenzamide, A new synthetic method of this compound is introduced below., Computed Properties of C7H6INO

General procedure: To a solution of 2-iodobenzamide (3) or 2-bromonicotinamide (6) (2.0 mmol) in DMSO (3 mL), was added aldehyde (2.2 mmol), NaN3 (260 mg, 4.0 mmol), CuBr (29 mg, 0.2 mmol), and l-proline (46 mg, 0.4 mmol). The reaction mixture was stirred at 80 C under air. After disappearance of the reactant (monitored by TLC), water (30 mL) was added to the mixture, and then extracted with ethyl acetate (15 mL) for three times. The extraction was washed with saturated NaCl solution, dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using petroleum ether/ethyl acetate (10:1 to 3:1) as the eluent to give the desired products 5 or 7.

The synthetic route of 3930-83-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Ting; Chen, Minglu; Yang, Lei; Xiong, Zhengxin; Wang, Yongwei; Li, Fei; Chen, Dongyin; Tetrahedron; vol. 72; 6; (2016); p. 868 – 874;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 103962-05-6, 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.

A mixture of 220( .613g, 9.Olmmol), Cs2C03 (4.40g. 13.5 Immol), 224(2Og, 9.Olmmoi) andCu(OAc)2 (0. 16g) in 20mL DMF. The mixture was heated at 120¡ãC for the appropriate time andsubsequent cooling, the reaction mixture was diluted with saturated aqueous ammonium chloride.Products were isolated by extraction with EA. The organic layer was dried over anhydrousNa2SO4, filtered, and concentrated. Products 225 were purified by silica gel columnchromatography (1 40g, yield: 68percent).

The synthetic route of 103962-05-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; HUA MEDICINE (SHANGHAI) LTD.; CHEN, Li; JIN, Xiaowei; (176 pag.)WO2017/117708; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 51560-21-5, These common heterocyclic compound, 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene, 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.

Under nitrogen, the 7.8g 2,5-diiodo-1,4-methoxybenzene was dissolved in 50mL of dichloromethane, and at -78 condition, to the solution was added dropwise 5.58mL three boron bromide. After completion of the dropwise addition, stirred for 16 hours at room temperature, the solid was suction filtered to produce a large number, and dried in vacuo to give a white solid which is 2,5-diiodo-1,4-bis(hydroxy)benzene. Among these, 2,5-diiodo-1,4-di(methoxybenzene, boron tribromide in methylenechloride and the molar ratio of 1: 3:40;

The synthetic route of 51560-21-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shaanxi Normal University; Fang, Yu; Sun, xiaohuan; Cui, Hong; Qi, yanyu; Liu, ke; Wang, Gang; Chang, xingmao; (21 pag.)CN104031108; (2016); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 1878-94-0,Some common heterocyclic compound, 1878-94-0, name is 2-(4-Iodophenoxy)acetic acid, molecular formula is C8H7IO3, 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 Example 10 Synthesis of Compound 10 (0209) (0210) A vial was charged with a carboxylic acid (371 mg, 1 equiv.), a solvent (1 mL of a solution of 200 g N-oxybenzotriazole in 1 L of DMF), and an amine (254 mg, 1 equiv.). To the stirred reaction mixture, EDC was added (228 mg, 1.1 equiv.). In case the reaction mixture became highly viscous, some more DMF was added. In case the reaction mixture was a homogeneous solution, it was kept at room temperature for 72 hrs. Otherwise, the reaction mixture was sonicated at room temperature for 5 days. The reaction mixture was diluted with 1% aqueous sodium phosphate solution until the vial was full. Then the vial was sonicated. In case a crystalline precipitate was formed, the vial was subjected to the filtration. In case an oily product was formed, the product was dissolved in methanol and precipitated by an addition of 4% hydrochloric acid. Alternatively 2-propanol (1 mL) was mixed with the crude product and the mixture was sonicated. Then the solution was diluted with 5% aqueous sodium hydrogen carbonate solution (the procedure repeated 2-3 times if necessary). The crude product was purified by chromatography (silica gel, chloroform: 2-propanol=4:1) The yield was 506 mg (84%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(4-Iodophenoxy)acetic acid, its application will become more common.

Reference:
Patent; THE UNIVERSITY OF TOKYO; RIKEN; KADOWAKI, Takashi; YAMAUCHI, Toshimasa; IWABU, Miki; IWABU, Masato; YOKOYAMA, Shigeyuki; HONMA, Teruki; (158 pag.)US2016/214967; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com