Category: 13101-40-1

Some common heterocyclic compound, 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, molecular formula is C6H3BrClI, 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: 13101-40-1

A mixture of 1-bromo-3-chloro-5-iodobenzene (1.5 g, 4.73 mmol), 4-(2,6-diisopropylphenyl)-1H-pyrazole (1.133 g, 4.96 mmol), 63 copper chloride dihydrate (0.161 g, 0.945 mmol), and 64 cesium carbonate (3.08 g, 9.45 mmol) was vacuumed and back-filled with nitrogen several times. 65 DMF (20 ml) was added to the reaction mixture and heated at 120 C. for 18 h. Cooled down and partitioned between EA and water and extracted with EA with a bit of NH4OH(aq). The organic portion was washed with brine and concentrated. Chromatographed on silica (DCM/Hep=2/1). Obtained white solid (73%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 13101-40-1, its application will become more common.

Reference:
Patent; UNIVERSAL DISPLAY CORPORATION; CHEN, Hsiao-Fan; (99 pag.)US2019/165284; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 13101-40-1, 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. 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Potassium carbonate (as 2 M aqueous solution, 2 eq.) was degassed with nitrogen for 30 min. Dioxane (976 ml) was also degassed with nitrogen for 30 min. The THF flask was then charged with corresponding 9-phenanthreneboronic add (10 mmol, 1.32 eq.), previously synthesized formula 6 intermediate (78 g, 1 eq.) and tetrakis(triphenylphosphin)palladium(o) (0.035 eq.) under a positive nitrogen pressure. The degassed potassium carbonate solution was added, nitrogen purged reflux condenser was attached to the flask and a reaction mixture heated to 65 C with stirring for 48 h. The mixture was allowed to cool down to the room temperature, dioxane was evaporated. Extraction with 1.75 L chloroform was performed. After washing the organic layer with 5 x 250 mL water, it was dried over MgSOq and filtered over silicagel layer. Evaporation almost to dryness followed by hexane addition provided a precipitate that was still colored. Further washing with Na2S20s sat. aqueous solution afforded 49.2g (54%) product, m/z 366, 368 [M]+

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-3-chloro-5-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NOVALED GMBH; SCHULZE, Benjamin; CARDINALI, Francois; SCHOLZ, Johannes; (74 pag.)WO2019/201621; (2019); A1;,
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. 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H3BrClI

Weigh 1-bromo-3-chloro-5-iodobenzene and raw material A, dissolve it with toluene, and add Pd2(dba)3, tri-tert-butylphosphine and sodium t-butoxide; The mixed solution of the above reactants is reacted at a reaction temperature of 95 to 110 C under an inert atmosphere for 10 to 24 hours. Cooling and filtering the reaction solution, and the filtrate is steamed and passed through a silica gel column to obtain an intermediate M; The molar ratio of the starting material A to 1-bromo-3-chloro-5-iodobenzene is 1: (1.0-1.5), and the molar ratio of the Pd2(dba)3 to the raw material A is (0.005-0.01): 1 ,The molar ratio of the tri-tert-butylphosphine to the starting material A is (0.005-0.01): 1,The molar ratio of the sodium tert-butoxide to the raw material A is (1-3): 1, The toluene is used in an amount of from 100 to 150 ml of toluene per 0.01 mol of 1-bromo-3-chloro-5-iodobenzene

According to the analysis of related databases, 13101-40-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jiangsu March Optoelectric Technology Co., Ltd.; Zhao Sijie; Wang Fang; Xie Dandan; Wu Xiuqin; Zhang Zhaochao; (45 pag.)CN109912431; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 13101-40-1,Some common heterocyclic compound, 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, molecular formula is C6H3BrClI, 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.

(1) In a 250ml three-neck flask, nitrogen protection, was added 0.012mol 1- bromo-3-chloro-5-iodobenzene, 0.01 mol starting material A-3,150ml of toluene stirred and mixed, followed by addition of 5×10-5mol Pd2(dba)3,. 5 × 10-5mol tri-tert-butyl phosphate, 0.03 mol of sodium tert-butoxide and heated to 105 deg.] C, the reaction was refluxed for 24 hours, and sampling showed no residual amino compound, the reaction was complete; cool to room temperature, filtered, The filtrate was rotary evaporated until no fraction, through neutral silica gel column chromatography to give intermediate M-8, purity 99.8%, yield 89.6%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-3-chloro-5-iodobenzene, its application will become more common.

Reference:
Patent; Jiangsu March Optoelectric Technology Co., Ltd.; Zhao Sijie; Wang Fang; Xie Dandan; Wu Xiuqin; Zhang Zhaochao; (47 pag.)CN109836339; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 13101-40-1, 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 13101-40-1 as follows.

Nitrogen was passed into the three-necked flask equipped with mechanical stirring, thermometer and condenser,Add 100.0 mL of toluene, compound 5b-4 (20 mmol),Starting material 3-chloro-5-bromoiodobenzene (ie compound 5b-5, 21 mmol),Potassium carbonate (40 mmol), 20 mL ethanol, 20 mL water. Start stirring,The temperature was raised to 50 C, and tetrakistriphenylphosphine palladium (0.2 mmol) was quickly added.Continue heating to reflux state for 6h, pour into 100mL water with stirring,After standing, the liquid was separated, and the aqueous phase was extracted with 50 mL of toluene, and the organic phases were combined.Dry with 10g of anhydrous sodium sulfate, filter, and concentrate the filtrate (70 , -0.09MPa),Concentrate to distill off without solvent, add 50ml n-heptane,Filtration gave compound 5b-6 (17 mmol) in 85% yield.

According to the analysis of related databases, 13101-40-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanxi Laite Optoelectric Materials Co., Ltd.; Wang Jinping; Xue Zhen; Chen Zhiwei; (47 pag.)CN110981860; (2020); 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. 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Bromo-3-chloro-5-iodobenzene

In a 250mL three-necked flask, nitrogen is introduced.Add 0.02molRaw material I, 150ml DMF, 0.022mol raw material II,0.0002 mol of palladium acetate, stirred,Then add 3mL of 0.01mol/mL K3PO4 aqueous solution,The reaction was heated under reflux at 150 C for 12 hours.Sampling the plate and the reaction is complete.Cool naturally, add 100mL water,The mixture was filtered and the filter cake was dried in a vacuum oven.The residue obtained was purified by silica gel column to giveRaw material A-1;

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; Jiangsu March Optoelectric Technology Co., Ltd.; Lu Ying; Wang Fang; Xie Dandan; Wu Xiuqin; Zhang Zhaochao; (39 pag.)CN109928911; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 13101-40-1, name is 1-Bromo-3-chloro-5-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 13101-40-1, COA of Formula: C6H3BrClI

The following reagents and solvents were charged into a reaction vessel. Compound J20: 1.44 g (5.00 mmol) Compound J21: 2.11 g (6.33 mmol), Toluene: 10 ml, Ethanol: 10 ml, 10 mass % Sodium carbonate aqueous solution: 20 ml. Next, 288 mg (0.0025 mmol) of tetrakis triphenylphosphine palladium(0) were added to the reaction solution and then the reaction solution was heated to 90 C. and stirred at the temperature (90 C.) for 5 hours. After the completion of the reaction, the reaction solution was cooled and then an organic layer was extracted with toluene. Next, the extracted organic layer was dried and then the solvent was removed by distillation under reduced pressure to provide a coarse product. Next, the coarse product was purified by silica gel column chromatography (developing solvent; heptane_chloroform=2:1) to provide 1.55 g (yield: 72%) of Compound J22.

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-3-chloro-5-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Canon Kabushiki Kaisha; Nishide, Yosuke; Yamada, Naoki; Kamatani, Jun; Ishii, Ryuji; Kajimoto, Norifumi; Ito, Takayuki; Mizuno, Nobutaka; Ishige, Koichi; Saitoh, Akihito; (71 pag.)US9755165; (2017); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 13101-40-1, A common heterocyclic compound, 13101-40-1, name is 1-Bromo-3-chloro-5-iodobenzene, molecular formula is C6H3BrClI, 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 100 mL two-necked flask was dried in the oven and charged with 1-bromo-3-chloro-5-iodobenzene (2.02 g, 6.37 mmol) and NiCl2(PPh3)2 (0.208 g, 0.318 mmol). The reaction mixture was vacuum and back-filled with nitrogen. Diethyl ether (20 ml) and (2,4,6-triisopropylphenyl)magnesium bromide in THF (12.73 ml, 6.37 mmol) was added and heated at 55 C. for 18 hrs. The reaction mixture was then cooled down and coated on celite and chromatographed on silica (Heptane) (1.74 g, 69%).

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.