Month: June 2021

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 16518-62-0 as follows. Safety of 3-Bromo-N,N-dimethylaniline

N,N-Diallyl-3-bromo-4-(2-bromo-4-(dimethylamino)benzyl)aniline (7) A solution of 3-bromo-N,N-dimethylaniline (7.54 g, 37.7 mmol) and 3-bromo-N,N-diallylaniline (9.51 g, 37.7 mmol) in glacial AcOH (250 mL) was treated with a 37 wt. percent solution of formaldehyde in H2O (30 mL). The resultant suspension was stirred at 80° C. for 2 h. After cooling to room temperature, the volatiles were removed under reduced pressure. The syrupy residue was dissolved in CH2Cl2 (100 mL), washed with sat. Na2CO3 (100 mL*2) and brine (100 mL), dried (Na2SO4), and concentrated under reduced pressure to afford a light brown syrup (16.9 g). 1H NMR analysis indicates that this mixture consists of approximately 30percent the desired product. The inseparable mixture was used in the subsequent step without further purification. 1H NMR (400 MHz, CDCl3): delta 6.91 (d, J=2.8 Hz, 2H), 6.82 (d, J=8.1 Hz, 2H), 6.55 (dd, J=2.8, 8.8 Hz, 2H), 5.78-5.87 (m, 2H), 5.14-5.20 (m, 4H), 3.98 (s, 2H), 3.85-3.87 (m, 4H), 3.15 (s, 6H).

According to the analysis of related databases, 16518-62-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CHANG, Christopher J.; VAN DE BITTNER, Genevieve V.; HIRAYAMA, Tasuku; CHAN, Jefferson; US2014/51863; (2014); 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. 1073-39-8, name is 3-Bromobicyclo[4.2.0]octa-1,3,5-triene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 1073-39-8

General procedure: In a 100 mL round-bottom flask, 1,2-dibromoethane (0.3 mL), magnesium (1.9 g, 80 mmol), and dry THF (5 mL) were added and stirred at ambient temperature for 30 min under nitrogen. Then 3-chloropropylmethyldichlorosilane (9.5 mL, 60 mmol) in THF(45 mL) was added dropwise over a period of 15 min and the reaction mixture was heated to 50 C for another 2 h. In another flask, magnesium (1.44 g, 60 mmol) and a grain of iodine were added. Then 4-bromobenzocyclobutene (9.15 g, 50 mmol) in 30 mL of dry THF was slowly added dropwise over a period of 2 h under nitrogen atmosphere. The reaction mixture was heated to 50 C and stirred continuously for 1 h. Resulted solution was added to the first flask. The reaction temperature was elevated to 50 C and kept overnight. Then the solution was poured into 1 M aq. HCl and extracted with hexane. The organic layer was washed twice with water and dried over anhydrous sodium sulfate. After removing the solvents by rotary evaporation, the residual oil was purified by silica-gel column chromatography (petroleum ether) to give the colorless oil (30.5 mmol, 5.74 g) in 61% yield.

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 1073-39-8.

Reference:
Article; Hu, Huan; Liu, Lili; Li, Zheng; Zhao, Cuijiao; Huang, Yawen; Chang, Guanjun; Yang, Junxiao; Polymer; vol. 66; (2015); p. 58 – 66;,
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. 112279-72-8, name is 4-Bromo-2,3-difluoroaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 112279-72-8

Benzyl chloroformate (1.1 mL, 7.5 mmol) was added dropwise with stirring to the Intermediate 52 (1.0 g, 4.8 mmol) in 10% aq. NaOH (15 mL)) and THF (30 mL) at ca. 0 C. The reaction mixture was stirred at r.t. for ca. 6 h. The reaction was quenched with 10% NH4Cl solution and extracted with DCM (2×50 mL). Combined organic layers were washed with brine, dried (Na2SO4), and concentrated under vacuum. The residue was purified by preparative TLC (10% ethyl acetate/petroleum ether) to give the product as a white solid. 1H NMR (400 MHz, CDCl3): 7.88 (m, 1H); 7.40 (m, 5H); 6.90 (m, 1H); 5.25 (s, 2H).

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; Gordeev, Mikhail Fedorovich; US2009/48305; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 185122-74-1, 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 185122-74-1 as follows.

At 0 0C and under protective atmosphere, a solution of 2-propanesulfonyl chloride (1 1.87 mL, 121 mmol) in DCM (121 mL) was added gradually to a solution of 5-bromo-2,3- dihydro-7/-/-inden-1 -amine (12.8 g, 60.4 mmol) and 1 ,8-diazabicyclo[5.4.0]undec-7-ene (4.83 mL, 32.1 mmol) in dichloromethane (300 mL). The reaction was stirred at rt overnight. The reaction mixture was washed with 1 N KHSO4 (1x) and sat NaHCOs (2x) before being dried on IS^SO4 and solvent evaporated in vacuo to afford a green oil. Purification by column chromatography (25% EtOAc in hept) afforded the title compound as a white solid (6.0 g, 18.9 mmol, 31 %). MS (ESI) : m/z [M – H]”317.0.

According to the analysis of related databases, 185122-74-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; N.V. ORGANON; WO2009/147167; (2009); 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. 418762-26-2, name is 4-Bromo-2-fluoro-5-methylaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 418762-26-2

To a stirred solution of 4-(2-(benzyloxy)ethoxy)-l-methyl-lH-pyrazole-5-carbonyl chloride (0.9 g, 3.05 mmol, 1 equiv) and 4-bromo-2-fluoro-5-methylaniline (0.6 g, 3.05 mmol, 1 equiv) in DCM was added Et3N (0.5 g, 4.58 mmol, 1.5 equiv) at 0 C under nitrogen atmosphere. The resulting solution was stirred for 30 min. The reaction was quenched with water at room temperature. The aqueous layer was extracted with CH2CI2 and the organic layer was concentrated under reduced pressure to give the title compound (1 g, 70.84%) as a white solid. LC-MS: (ES, m/z): [M+H]+ 462.

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; IDEAYA BIOSCIENCES, INC.; ALAM, Muzaffar; BECK, Hilary, Plake; DILLON, Michael, Patrick; GONZALEZ-LOPEZ, Marcos; SUTTON, James, Clifford, Jr.; (248 pag.)WO2019/156987; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 17247-58-4, name is (Bromomethyl)cyclobutane, belongs to bromides-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 17247-58-4, SDS of cas: 17247-58-4

Potassium ie tert-butoxide 1N in tetrahydrofuran (5.75 mL, 5.75 mmol) was added to a suspension of 5-bromo-2(1 H)-pyridone (1.00 g, 5.75 mmol) in dimethoxyethane (10 mL). After 30 minutes stirring at room temperature, potassium carbonate (0.56 g, 4.02 mmol) and (bromomethyl)cyclobutane (1 .29 mL, 1 1 .49 mmol) were added and the reaction mixture was refluxed for 24 hours. The resultant precipitate was filtered and rinced with ethyl acetate (20 mL). The filtrate was successively washed with water (20 mL) and brine (20 mL), then dried over sodium sulfate and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (dichloromethane/ethyl acetate: 100/0 to 80/20) to provide 5-bromo-1 – (cyclobutylmethyl)-1 ,2-dihydropyridin-2-one (30a) ( 1 .10 g, 4.54 mmol, 79%). 1H NMR (400 MHz, CDCl3) delta 1.72-1.85 (m, 2H), 1 .85-1.97 (m, 2H), 2.01 -2.12 (m, 2H), 2.77 (septuplet, J = 7.5 Hz, 1 H), 3.92 (d, J = 7.5 Hz, 2H), 6.47 (d, J = 9.5 Hz, 1 H), 7.31 (dd, J = 2.7 Hz, J = 9.5 Hz, 1 H), 7.34 (d, J = 2.7 Hz, 1 H). MS m/z ([M+H]+) 242/244.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (Bromomethyl)cyclobutane, and friends who are interested can also refer to it.

Reference:
Patent; LABORATOIRE BIODIM; BENAROUS, Richard; CHEVREUIL, Francis; LEDOUSSAL, Benoit; CHASSET, Sophie; LE STRAT, Frederic; WO2014/57103; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 393-36-2, 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. 393-36-2, name is 4-Bromo-3-(trifluoromethyl)aniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of [6-CHLORO-4-ISOPROPYL-N- (TETRAHYDROPYRAN-4-YLMETHYL)-NICOTINAMIDE] (Description 8) (100mg), [4-BROMO-3-TRIFLUOROMETHYL-] (ex Lancaster, 162mg), [METHANESULFONIC] acid [(44NL)] in 1,4-dioxane [(1MI)] was irradiated under microwave conditions at [180FOR] 30 minutes. After removal of the 1,4-dioxane under reduced pressure, the mixture was partitioned between ethyl acetate [(5ML)] and brine [(2ML)] and the aqueous layer separated. The organic layer was evaporated under reduced pressure and the residue purified using the Biotage Horizon system. Purification afforded the title compound as a white solid (47mg). NMR [(DMSO-D6)] [No.1. ]16-1.23 (8H, d, m), 1.60-1. 63 (2H, d), 1.75 (1H, m), 3.10 (2H, t), 3.28 (2H, t), 3.41 (1H, m), 3.85 (2H, d), 6.80 (1H, s), 7.73 (1H, d), 7.83 (1H, d), 8.16 (1H, s), 8.38-8. 42 (2H, m), 9.70 (1H, s). LC/MS t = 3.5 min, [MH+] 500, consistent with molecular formula [C22H2579BR F3N302]

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, 4-Bromo-3-(trifluoromethyl)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXO GROUP LIMITED; WO2004/29026; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 626-39-1, 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. 626-39-1, name is 1,3,5-Tribromobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1,3,5-tribromobenzene (3.11 g, 10 mmol), pyridine-3-boronic acid (2.71 g, 22 mmol), tetrakis(triphenylphosphine)palladium(1.56 g, 1 mmol) and potassium carbonate (5.52 g, 40 mmol) were added to the reaction flask.The nitrogen was exchanged three times (10 min/time). Injecting solvent under nitrogen protection(toluene: ethanol: water = 8:1:1), after the completion of the injection, the reaction was refluxed at 120 C for 8 h;Extract, concentrate, make powder,Purification by column chromatography gave white solid product 1 in 65% yield.

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, 1,3,5-Tribromobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; South China University of Technology; Tang Benzhong; Zhao Zujin; Hu Shimin; Qin Anjun; Hu Rongrong; Wang Zhiming; (24 pag.)CN109593079; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 418762-26-2, name is 4-Bromo-2-fluoro-5-methylaniline, molecular formula is C7H7BrFN, 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 C7H7BrFN

To a solution of 4-bromo-2-fluoro-5-methylaniline (1.10 g, 5.39 mmol), ethyl 4-(3-methylbutanoyl)benzoate (1.26 g, 5.39 mmol) and Et3N (2.25 ml, 16.2 mmol) in DCM (100 ml) was added TiCl4 (2.7 ml, 2.7 mmol) dropwise and the reaction was monitored by TLC. The mixture was kept stirring at room temperature for 16 h, then 5N NaOH was added to adjust pH=14, extracted with DCM and the organic layer was washed with brine, dried and concentrated. The resulting residue was used for the next step reaction directly.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 418762-26-2, its application will become more common.

Reference:
Patent; Janssen Pharmaceutica NV; Gaul, Micheal; Xu, Guozhang; Zhao, Bao-Ping; (53 pag.)US2018/64686; (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. 7073-94-1, name is 1-Bromo-2-isopropylbenzene, A new synthetic method of this compound is introduced below., COA of Formula: C9H11Br

l-Bromo-2-/-propylbenzene (0.199 g, 1.00 mmol), (CyPF-Z-Bu)PdCl2 (7.30 mg, 1.00 x lO’2 mmol), and LiNH2 (0.230 g, 10.0 mmol) in 2.0 mL DME gave 0.109 g (81%) of 2-/-Propylaniline as a solid; Bromo-2-/-propylbenzene (1.99 g, 100 mmol) were weighed into a 100 mL round bottom flask with a stirring bar. DME (20.0 mL) was then added. The flask was sealed with a cap and wrapped tightly with electrical tape. The reaction mixture was stirred for 24 h at 90 0C. The reaction mixture was allowed to cool to room temperature before pouring into ice water (50.0 mL). To this mixture was added aqueous HCl (100 mL, 1.0 M). The mixture was stirred at room temperature for 5 min and was then neutralized with a saturated solution of NaHCO3 (50.0 mL). After extraction with CH2Cl2 (3 x 50.0 mL), the organic layer was separated and dried over MgSO4. The solvent was evaporated, and the crude product isolated by column chromatography, eluting with hexane/ethyl acetate (70/30) to give 1.11 g (82%) of 2-/-rhoropylaniline as a solid.

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; YALE UNIVERSITY; WO2007/109365; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary