Month: March 2021

Related Products of 402-43-7, 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. 402-43-7, name is 1-Bromo-4-(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: der nitrogen atmosphere in a glovebox, a stir bar, an aryl halide (0.40 mmol, 1.0 equiv.), quinuclidine (0.60 mmol, 1.5 equiv., 66.7 mg), and 1 mL of DMAc solution containing dissolved NiBr2.3H2O (0.02 mmol, 0.05 equiv., 5.5 mg) was added to a 0.5 dram glass vial. The glass vial was then capped using a screw cap equipped with a PTFE/silicone septum and sealed with a strip of PARAFILM. The capped vial was then brought out of the glovebox and liquid amine (degassed, 0.60 mmol, 1.5 equiv.) was added via a HAMILTON syringe. Solid amines were weighed and added inside the glovebox. The capped glass vial containing the reaction mixture was then placed in a 3D-printed vial holder and subjected to 365 nm LED irradiation with fan cooling to maintain the vial at room temperature. After the time specified in the reaction schemes, the reaction mixture was washed with water, extracted with EtOAc or DCM and concentrated under vacuum. Purification of the crude product by flash chromatography on silica gel using the indicated solvent system afforded the desired product

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-4-(trifluoromethyl)benzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Colorado State University Research Foundation; Miyake, Garret; Lim, Chern-Hooi; Kudisch, Max; Liu, Bin; (41 pag.)US2019/345122; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 4101-68-2, These common heterocyclic compound, 4101-68-2, name is 1,10-Dibromodecan, 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 atmosphere, compound 7 (1.23 g, 1.65 mmol), 1,10-dibromodecane (2.97 g, 9.9 mmol), potassium hydroxide (0.43 g, 6.6 mmol), tetrabutylammonium bromide , 0.495 mmol) was added to dichloromethane (10 ml) and water (6.5 ml), and the mixture was stirred at room temperature for 24 hours. The mixture was allowed to stand for several minutes. The aqueous layer and the organic layer were separated, and methanol (30 ml) was added to the organic layer. The precipitate was filtered and purified by silica gel column chromatography (eluent ethyl acetate / petroleum ether, volume ratio 1: 30-1: 20) to give a colorless solid (1.41 g) in 89% yield.

The synthetic route of 4101-68-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guilin University of Technology; Kong, Xiangfei; Wang, Guixia; Xia, Liting; Su, Jian; Zhang, Haifeng; (19 pag.)CN105541616; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 583-70-0, 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. 583-70-0, name is 2,4-Dimethylbromobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 2: to a suspension of magnesium powder (239 mg, 9.79 mmol) in dry THF(small amount) was added dropwise 1 -bromo-2,4-dimethylbenzene (1.64 g, 8.86mmol) diluted in dry THF (20 mL) and the reaction was heated at 40C. Aftercompletion of Grignard reagent, 2-methyl-N-[(5-methylfuran-2-yl)methylidene]propane-2-sulfinamide (995 mg, 4.66 mmol) diluted in THF (10mL) was added to the solution. The reaction mixture was stirred at rt overnight.Water was added to quench the reaction. The two layers were partitionated andthe organic layer was dried over Mg504, filtered and the solution wasconcentrated under reduced pressure. The crude material was purified by silicagel column chromatography using a gradient of hexanes/EtOAc ([5:1] to [4:1]) to afford N-[(2,4-di methyl phenyl)(5-methylfuran-2-yl)methyl]-2-methylpropane-2- sulfinamide (1 .27 g, 85%) as yellowish oil

The synthetic route of 2,4-Dimethylbromobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GENFIT; DELHOMEL, Jean-Francois; PERSPICACE, Enrico; MAJD, Zouher; PARROCHE, Peggy; WALCZAK, Robert; BONNET, Pascal; FOGHA, Jade; (82 pag.)WO2018/138354; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C14H21Br

In a 500 ml glass reaction vessel, 17.9 g (66.5 mmol) of 1-bromo-3,5-di-tert-butylbenzene,200 ml of dimethoxyethane (DME) was added,dry ice-It was cooled to -78 ¡ã C. in a methanol bath.Here, 1.65 mol / LA solution of tert-butyllithium-n-pentane80.6 ml (132 mmol)Was added dropwise,Stir for 2 hours as it was. While being cooled at -78 ¡ã C.,18.0 ml (78 mmol) of triisopropylborate was added dropwise.After the dropwise addition, the mixture was stirred for 17 hours while gradually returning to room temperature. After adding a solution of 38 g of tripotassium phosphate / 100 mL of distilled water and hydrolyzing,10.0 g (51.3 mmol) of 4-bromo-indene,1.30 g (4.96 mmol) of triphenylphosphine and 1.80 g (2.56 mmol) of dichlorobis (triphenylphosphine) palladium were successively added,After removing the low boiling fraction,And heated at 85 ¡ã C. for 6 hours.After allowing to cool, the reaction solution was poured into 100 ml of distilled water, transferred to a separating funnel and extracted with n-hexane three times, 10 ml of concentrated hydrochloric acid was added to the hexane solution at room temperature, and the mixture was stirred at room temperature for 30 minutes to obtain a palladium compound After precipitation, the mixture was filtered through filter paper, and the filtrate was washed three times with saturated brine and distilled water, and dried over sodium sulfate. The sodium sulfate was filtered, the solvent was distilled off under reduced pressure, dissolved in hexane / diisopropyl ether = 10: 1, and filtered through a silica gel column to give 4- (3,5-tert-butylphenyl) indene, 15.6 g of a pale yellow oil was obtained (yield 100percent).

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 22385-77-9.

Reference:
Patent; Japan Polyethylene Corporation; Japan Polypropylene Corporation; Itagaki, Koji; Sakuragi, Tsutomu; (20 pag.)JP2015/110528; (2015); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 332-42-3, These common heterocyclic compound, 332-42-3, name is 1-Fluoro-4-(2-bromoethyl)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.

To a mixture of 5-(1H-pyrazol-3-yl)-thiophene-2-carbonitrile [300mg, 1.72mmol, Reference Example 3 (b) ], potassium carbonate [(500MG,] 3. [6MMOL)] and [N, N-] [DIMETHYLFORMAMIDE] (4ml) was added 1- (2-bromoethyl)-4-fluoro-benzene (566mg, 3.4mmol). The resulting mixture was heated to [80C] and stirred overnight. The reaction mixture was then quenched in water and extracted with diethyl ether. The organic layer was dried (MgSO4), concentrated, and then subjected to flash column chromatography using a mixture of cyclohexane and ethyl acetate [(8] : 2, v/v) as eluent, to provide [5-{1-[2-(4-] [FLUORO-PHENYL !-ETHYL]-1 H-PVRAZOL-3-YL}-THIOPHENE-2-CARBONITRILE.]

The synthetic route of 332-42-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARGENTA DISCOVERY LIMITED; WO2004/13130; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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 327-51-5 as follows. COA of Formula: C6H2Br2F2

Compound A-14 (24.6 g, 74 mmol), 1, 4-dibromo-2, 5-difluorobenzene (20 g, 74 mmol), and a 2 M aqueous solution of Na2CO3 (75 mL, 150 mmol), DME (150 mL), toluene (150 mL), and Pd [PPh3]4 (4.3 g, 3.7 mmol) were loaded into a three-necked flask, and the mixture was refluxed under an Ar atmosphere for 8 hours. After the completion of the reaction, the resultant was cooled to room temperature. The resultant sample was transferred to a separating funnel, and water (100 mL) was charged into the funnel. Then, the mixture was extracted with CH2Cl2. The extract was dried with MgSO4, and was then filtrated and concentrated. The resultant sample was purified by silica gel column chromatography, whereby a white solid was obtained in an amount of 21 g in 60% yield. FD-MS C24H13BrF2N2O2: theoretical value 479, observed value 479

According to the analysis of related databases, 327-51-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2301921; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 54962-75-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 54962-75-3 name is 3-Bromo-5-(trifluoromethyl)aniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

A mixture of 3-bromo-5-(trifluoromethyl)aniline (0.48 g, 2.0 mmol), 4-cyclopropyl-lH- imidazole (0.26g, 2.4 mmol), K2CO3 (0.35g, 2.5 mmol), CuI (57 mg, 0.30 mmol), and 8- hydroxyquinoline (44 mg, 0.30 mmol) in dry DMSO (2 mL) in a microwave tube was cooled to -78deg;C, and degassed by vacuum and refilled with N2 for three times. The mixture was heated at1200C overnight. The mixture was cooled to 40-500C and 14% aq. NH4OH was added. The mixture was stirred at 40-500C for 1 h. After cooling, the mixture was diluted with water, and extracted with ethyl acetate (3×15 mL). The combined organic layers were dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column (5% MeOH in CH2Cl2) to afford the crude product (0.41 g). LCMS: (M+H)+= 268.3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Bromo-5-(trifluoromethyl)aniline, and friends who are interested can also refer to it.

Reference:
Patent; SYNTECH SOLUTION LLC; CHEN, Yongsheng; WO2010/96395; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 103273-01-4, name is 2-Bromo-4-(tert-butyl)aniline, This compound has unique chemical properties. The synthetic route is as follows., Safety of 2-Bromo-4-(tert-butyl)aniline

Prepared according to a modified literature procedure.14 To a solution of 2-bromo-4-(tert-butyl)aniline (11) (684 mg, 3.00 mmol, 1.0 eq.) in acetonitrile (6 mL) at room temperature, was added methyl acrylate (675 muL, 7.50 mmol, 2.5 eq.), palladium acetate (135 mg, 0.6 mmol, 20 mol %), tri-o-tolylphosphine (640 mg, 2.10 mmol, 0.7 eq.) and triethylamine (1.67 mL, 12.0 mmol, 4.0 eq.).The reaction was heated to reflux for 9 hours, cooled to room temperature and concentrated under reduced pressure. The crude residue was dissolved in ethyl acetate, washed with water and the aqueous phase extracted with ethyl acetate. The combined organic phases were dried over magnesium sulphate and the solvent removed under reduced pressure. Purification by flash chromatography on silica gel (SiO2, petroleum ether 30-40: EtOAc 9:1-4:1) afforded the title compound as a yellow solid (531 mg, 2.28 mmol, 76 % yield).

According to the analysis of related databases, 103273-01-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Buckingham, Faye; Calderwood, Samuel; Checa, Begona; Keller, Thomas; Tredwell, Matthew; Collier, Thomas Lee; Newington, Ian M.; Bhalla, Rajiv; Glaser, Matthias; Gouverneur, Veronique; Journal of Fluorine Chemistry; vol. 180; (2015); p. 33 – 39;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 90267-03-1, name is 1-Bromo-3,5-diethylbenzene, A new synthetic method of this compound is introduced below., name: 1-Bromo-3,5-diethylbenzene

A mixture of N- ( 4- (methylsulfonyl ) benzyl ) -3, 4-dihydro-2H- (3804) 1.4-benzoxazine-7-carboxamide (0.028 g, 0.08 mmol), 1-bromo- (3805) 3.5-diethylbenzene (34 mg, 0.160 mmol), RuPhos Pd Gl (5.83 mg, 8.00 mumol), RuPhos (3.73 mg, 8.00 mumol) , NaOtBu (0.023 g, 0.240 mmol) and DME (1 mL) was heated at 130 C for 2 h under (3806) microwave irradiation. The reaction mixture was diluted with AcOEt (3 mL) and quenched with H20 (1 mL) , and stirred for 2 min. The organic layer was separated and then the aqueous layer was extracted with EtOAc (2 mL) . The combined organic layer was evaporated by blowing away with the air at 60 C. The residue was purified by preparative HPLC (Actus Triart C18, eluted with MeCN/10 mM NH4HCO3 aq. 5:95?100:0). Pure fractions were combined and concentrated by blowing away with the air at 60C to afford the title compound (23 mg, 0.0481 mmol, 60%).

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; TAKEDA PHARMACEUTICAL COMPANY LIMITED; YAMAMOTO, Satoshi; SHIRAI, Junya; KONO, Mitsunori; SHIOKAWA, Zenyu; YUKAWA, Tomoya; IMADA, Takashi; NEGORO, Nobuyuki; ODA, Tsuneo; SASAKI, Satoshi; NARA, Yoshi; SUZUKI, Shinkichi; SATO, Ayumu; ISHII, Naoki; SHIBUYA, Akito; NAKAGAWA, Yasuo; COLE, Derek; GIBSON, Tony; IVETAC, Anthony; SWANN, Steve; TYHONAS, John; (472 pag.)WO2018/30550; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 1195-33-1, name is 4-Bromobenzenesulfinic acid, A new synthetic method of this compound is introduced below., Computed Properties of C6H5BrO2S

Thionyl chloride (0.53 ml_) is added to an ice-cooled solution of 4- bromobenzenesulfinic acid (400 mg) in dichloromethane (15 ml_) under an argon atmosphere. The reaction mixture is stirred for 2 h at 0C, warmed to room temperature, and stirred for an additional 30 min. The mixture is concentrated and the residue is co-evaporated twice with toluene to give crude 4-bromobenzenesulfinic chloride, which is dissolved in tetrahydrofuran (3 ml_) and cooled to -78 C. n-Butyllithium (1 .6 M in hexane; 2.26 ml_) is added to 2,2,2-trifluoroacetamide (205 mg) in tetrahydrofuran (3 ml_) at -78 C and the reaction mixture is stirred for 10 min. The mixture is added to the 4-bromobenzenesulfinic chloride solution at -78 C and the reaction mixture is stirred for 1 h. The cooling bath is removed and the reaction is quenched by addition of water and brine. The aqueous layer is extracted with ethyl acetate and the combined extracts are washed with brine and concentrated in vacuo to give the title compound which is used for the next step without further purification. LC (method 1 ): tR = 0.92 min; Mass spectrum (ESI+): m/z = 314 [M-H]

The synthetic route of 1195-33-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; LANGKOPF, Elke; BLUM, Andreas; (89 pag.)WO2016/23789; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary