Tag: M.W=300-400

Synthetic Route of 160976-02-3, The chemical industry reduces the impact on the environment during synthesis 160976-02-3, name is 5-Bromo-1,3-difluoro-2-iodobenzene, I believe this compound will play a more active role in future production and life.

General procedure: A Schlenk tube was dried using heat gun under reduced pressure and filled with argon. The tube was charged with TPPO (69.5mg, 0.25mmol) and then the tube was evacuated and refilled with argon (¡Á3). To the tube were added THF (1mL), Me2Zn (0.6mL, 0.6mmol, 1.0M solution in hexane), and fluoroarene 1 (0.75mmol) at room temperature and then the tube was immersed in an oil bath. The reaction mixture was gradually warmed to 75C and stirred for 3h. The mixture was cooled to room temperature and allylic bromide (0.5mmol) was added. The resultant mixture was warmed to 75C and stirred for 16h. The reaction mixture was quenched with saturated aqNH4Cl solution followed by extraction with Et2O (¡Á3). Combined organic layer was washed with brine (¡Á1), dried over Na2SO4, and filtered. Volatiles were removed under reduced pressure and the residue was purified by flash column chromatography on silica gel to afford analytically pure product.

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-Bromo-1,3-difluoro-2-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kurauchi, Daisuke; Hirano, Keiichi; Kato, Hisano; Saito, Tatsuo; Miyamoto, Kazunori; Uchiyama, Masanobu; Tetrahedron; vol. 71; 35; (2015); p. 5849 – 5857;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 160976-02-3, A common heterocyclic compound, 160976-02-3, name is 5-Bromo-1,3-difluoro-2-iodobenzene, molecular formula is C6H2BrF2I, 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 a nitrogen atmosphere, to a three-necked flask equipped with a reflux condenser were added 2,6-difluoro-4-bromoiodobenzene (13.3g, 41.67mmol),9-methyl-9H-carbazole-4-ol (18g, 91.67mmol), potassium carbonate (23g, 166.68mmol) and 200mL N-methylpyrrolidone (NMP), and heated to reflux for 6h.After the reaction, the system was cooled to room temperature. After adding a large amount of water, a white precipitate is formed, which is collected by suction filtration. The precipitate was washed sequentially with water and methanol (50% (V / V)).Finally, the obtained filter cake was dissolved in an appropriate amount of dichloromethane and further purified by column chromatography (mobile phase: petroleum ether: dichloromethane = 3: 1 (V / V)),23g of white solid was obtained with 82% yield.

The synthetic route of 160976-02-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Jiuxian New Materials Co., Ltd.; Cui Linsong; Liu Xiangyang; Zhang Yexin; Chen Hua; (56 pag.)CN110981899; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 181765-86-6, 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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

2- bromo -4- chloro- 1- iodobenzene (87.5 g), 1- naphthylboronate (100 g), the tetrahydrofuran (1 L), the potassium carbonate (200.9 g) and water (720 mL) were put in 5 L three holes round bottom flask and it was stirred. The tetrakis (triphenylphosphine) palladium (0) (13.4 g) was put into the mixed solution and 80 heated for 24 hours. The reaction solution was cooled in a room temperature and it extracted in the dichloromethane. After it was dry to the magnesium sulfate it was the organic layer concentrated under reduced pressure and the solvent was removed. Material generated with the concentration were washed with the methanol and the powder I-2 of gray was obtained with 72 g.

The chemical industry reduces the impact on the environment during synthesis Methyl 5-bromo-2-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Daejoo Electronic Materials Co., Ltd.; Kim, Hyung Ho; Jeon, Young Min; Nam, Sang Jin; Kim, Soo Hyun; Kim, Min Young; Kim, Jun Woo; (29 pag.)KR2016/113488; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 31827-94-8, 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To 2.50 g (7.69 mmol) 2-bromo-1 -(4-iodo-phenyl)-ethanone in 30 mL ACN are added 1 .90 g (23.1 mmol) 4-methylimidazole and the mixture is stirred at rt for 48 h. After that time, the solvent is evaporated and the residue is taken up in EtOAc. The mixture is washed with water and brine (2x) and the organic layer is dried over magnesium sulphate. The solvent is evaporated and the residue is recrystallized from diethyl ether to yield the desired product.C12H11 IN2O (M = 326.13 g/mol)ESI-MS: 327 [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, 2-Bromo-1-(4-iodophenyl)ethanone, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ROTH, Gerald Juergen; FLECK, Martin; NEUBAUER, Heike; NOSSE, Bernd; WO2012/32014; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 181765-86-6, 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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: An oven-dried Schlenk tube equipped with a Teflon valve was charged with a magnetic stir bar, CuI (10 mg, 0.05 mmol, 10 mol%), K2CO3 (276 mg, 2.0 mmol), 1,10-phenanthroline (20 mg, 0.10 mmol, 20 mol%) and cyclic thiourea (0.5 mmol), 4 ? Molecular Sieves. The tube was evacuated and backfilled with N2 (this procedure was repeated 3 times). Under a counter flow of N2, methyl-2-iodobenzoate 1 (0.6 mmol) and DMF (2.0 mL) were added by syringe. The mixture was stirred at 100 ?C for 24h. After the reaction was completed, the mixture was directly passed through celite and rinsed with 30 mL of EtOAc. The combined filtrate was concentrated and purified by column chromatography on silica gel to give the pure product.Yellow Yellow solid; mp 152-154 C; 1H NMR (200 MHz, CDCl3) delta 8.31 (d, J = 2.0 Hz, 1H), 7.56 (dd, J1 = 8.6 Hz, J2 = 2.4 Hz, 1H), 7.07 (d, J = 8.6 Hz, 1H), 3.53-3.39 (m, 1H), 3.29-3.15 (m, 1H), 3.07-3.02 (m, 1H), 2.38-2.33 (m, 1H), 1.90-1.86 (m, 2H), 1.74-1.34 (m, 4H); 13C NMR (50 MHz, CDCl3) delta 160.9, 153.8, 136.4, 133.3, 131.1, 126.8, 126.2, 120.6, 71.9, 67.6, 31.0, 30.7, 29.9, 25.4, 24.9 ppm. Anal. Calcd. for C14H13BrN2OS: C 49.86, H 3.89, N 8.31; found: C 50.05, H 4.01, N 8.20; EI-MS: m/z = 336 (M+), 338(M+2).

The chemical industry reduces the impact on the environment during synthesis Methyl 5-bromo-2-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Article; Chen, Dingben; Wu, Jiashou; Yang, Jianguo; Huang, Ling; Xiang, Yubo; Bao, Weiliang; Tetrahedron Letters; vol. 53; 52; (2012); p. 7104 – 7107;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 63279-58-3, name is 1-Bromo-4-iodonaphthalene, 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 63279-58-3, Computed Properties of C10H6BrI

Synthesis Example 1 (Synthesis of a compound (AN-1)); Under the atmosphere of argon, 10 g of 1-bromo-4-iodonaphthalene and 6 g of 4-bromophenylboronic acid which were synthesized in accordance with conventional processes were dissolved into 150 ml of toluene, and 45 ml of a 2M aqueous solution of sodium carbonate was added. Then, 1 g of tetrakistriphenylphosphinepalladium was added, and the resultant mixture was heated under the refluxing condition for 7 hours. After one night, the formed organic layer was extracted with toluene, washed with water and a saturated aqueous solution of sodium chloride. The organic layer was dried with anhydrous sodium sulfate, and the solvent was removed by distillation. The residue was purified in accordance with the silica gel column chromatography (the solvent of development: toluene/hexane), and 6.3 g of 1-bromo-4-(4-bromophenyl)-naphthalene was obtained (the yield: 58percent). The obtained 1-bromo-4-(4-bromophenyl)naphthalene in an amount of 6 g was mixed with 10 g of 10-phenylathracene-9-boronic acid synthesized in accordance with a conventional process and 150 ml of DME. Then, 1.1 g of tetrakistriphenylphosphinepalladium and 50 ml of a 2M aqueous solution of sodium carbonate were added, and the atmosphere was purged with argon. After the resultant mixture was heated under the refluxing condition for 7.5 hours, the mixture was cooled by leaving standing, and formed crystals were separated by filtration. The separated crystals were washed with water, methanol and then heated toluene, and 8.3 g of the object compound (AN-1) was obtained as a light yellow solid substance (the yield: 70percent). When the obtained compound was examined in accordance with the field desorption mass spectroscopy (FDMS), it was found that m/z=708, which agreed with C56H36=708, and the above compound was identified to be Compound AN-1.

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-Bromo-4-iodonaphthalene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2003107; (2008); A1;,
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

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, Product Details of 628-77-3

Diiodopentane (0.63 niL, 4.21 mmol, 5 eq) and potassium carbonate (116 mg, 0.84 mmol, 1 eq) were added to a solution of phenol 54 (400 mg, 0.84 mmol) in acetone (4 mL, dried over molecular sieves). The reaction mixture was then warmed to 60C and stirred for 6 hours. Acetone was removed by rotary evaporation under reduced pressure. The resulting residue was subjected to flash column chromatography (silica gel; 50/50, v/v, hexane/ethyl acetate,). Pure fractions were collected and combined and excess eluent was removed to provide 55 in 90% yield. LC/MS, 3.90 min (ES+) m/z (relative intensity) 670.91 ([M]+, 100). 1H NMR (400 MHz, CDC13) delta 7.23 (s, 1H), 6.69 (s, 1H), 6.60 (s, 1H), 5.87 (d, / = 8.8 Hz, 1H), 5.83 – 5.68 (m, J = 5.6 Hz, 1H), 5.15 – 5.01 (m, 2H), 4.67 – 4.58 (m, 1H), 4.45 – 4.35 (m, 1H), 4.04 – 3.93 (m, 2H), 3.91 (s, 3H), 3.73 (td, / = 10.0, 3.8 Hz, 1H), 3.25 – 3.14 (m, / = 8.5, 7.0 Hz, 2H), 2.92 (dd, J = 16.8, 10.3 Hz, 1H), 2.38 (d, / = 16.8 Hz, 1H), 1.95 – 1.81 (m, 4H), 1.77 (s, 3H), 1.64 – 1.49 (m, 2H), 0.88 (s, 9H), 0.25 (s, 3H), 0.23 (s, 3H).

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, 1,5-Diiodopentane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MEDIMMUNE LIMITED; LLOYD, Christopher O.; MARWOOD, Rose; HOWARD, Philip; HARPER, III, John W.; HOLLINGSWORTH, Robert; KAMAL, Adeela; DIMASI, Nazzareno; GAO, Changshou; TOADER, Dorin; WANG, Fengjiang; GINGIPALLI, Lakshmaiah; WO2015/155345; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 112671-42-8, 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 112671-42-8 as follows.

Intermediate M3-a (3.7 g, 18.6 mmol) and 2-iodo-5-bromonitrobenzene (15.3 g, 46.7 mmol), sodium tert-butoxide(7.1 g, 74.4 mmol), 100 mL of toluene, nitrogen protection, Pd2 (dba) 3 (0.3 g),Tri-tert-butylphosphine (20ml, 10% in toluene), stirring, heating to 100 C reflux, reaction 12h, the reaction liquid was washed, the organic phase was concentrated, passed the silica gel column,The eluent is petroleum ether: ethyl acetate = 50:1, concentrated eluent,Intermediate M3-b (9.2 g, yield 82.7%) was obtained.

According to the analysis of related databases, 112671-42-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Beijing Dingcai Technology Co., Ltd.; Gu’an Dingcai Technology Co., Ltd.; Fan Hongtao; Zhang Yaguang; Zhang Xianghui; Ren Xueyan; (36 pag.)CN108440543; (2018); A;,
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. 628-77-3, name is 1,5-Diiodopentane, A new synthetic method of this compound is introduced below., Safety of 1,5-Diiodopentane

Diiodopentane (0.63 mL, 4.21 mmol, 5 eq) and potassium carbonate (116 mg, 0.84mmol, 1 eq) were added to a solution of phenol 54 (400 mg, 0.84 mmol) in acetone (4 mL,dried over molecular sieves). The reaction mixture was then warmed to 60C and stirred for 6 hours. Acetone was removed by rotary evaporation under reduced pressure. The resulting residue was subjected to flash column chromatography (silica gel; 50/50, v/v, hexane/ethyl acetate,). Pure fractions were collected and combined and excess eluent wasremoved to provide 55 in 90% yield. LC/MS, 3.90 mm (ES+) m/z (relative intensity)670.91 ([M], 100). ?H NMR (400 MHz, CDC13) oe 7.23 (s, 1H), 6.69 (s, 1H), 6.60 (s, 1H),5.87 (d, J= 8.8 Hz, 1H), 5.83 – 5.68 (m, J= 5.6 Hz, 1H), 5.15 – 5.01 (m, 2H), 4.67 -4.58(m, 1H), 4.45 -4.35 (m, 1H), 4.04 – 3.93 (m, 2H), 3.91 (s, 3H), 3.73 (td, J 10.0, 3.8 Hz,1H), 3.25 -3.14 (m, J= 8.5, 7.0 Hz, 2H), 2.92 (dd, J 16.8, 10.3 Hz, 1H), 2.38 (d, J16.8 Hz, 1H), 1.95 – 1.81 (m, 4H), 1.77 (s, 3H), 1.64 – 1.49 (m, 2H), 0.88 (s, 9H), 0.25 (s,3H), 0.23 (s, 3H).

The synthetic route of 628-77-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; STEM CENTRX, INC.; SPIROGEN SARL; TORGOV, Michael; HOWARD, Philip Wilson; WO2014/130879; (2014); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com