Month: July 2021

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. 937046-98-5, name is 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 937046-98-5

Intermediate 69A 7-( Prop- 1 -en-2-yl)pyrrolo[2, l-fj[l ,2,4]triazin-4-amine The starting material 7-bromopyrrolo[2, 1 -fj [ 1 ,2,4]triazin-4-amine was synthesized according to the procedure described in WO 2007/056170-A2 (Intermediate B). Under an argon atmosphere, 7-bromopyrrolo[2, 1 -f] [ 1 ,2,4]triazin-4-amine (426 mg, 2 mmol) and 4,4,5, 5-tetramethyl-2-(prop-l -en-2-yl)-l,3,2-dioxaborolane (420 mg, 2.5 mmol) were dissolved in a mixture of 1 ,2-dimethoxyethane (10 mL) and aqueous sodium carbonate solution (2 M, 4 mL). The reaction mixture was degassed, and 1 , 1 ‘-bis(diphenylphosphino)ferrocenepalladium(II) chloride (73 mg, 0.1 mmol) was added. After stirring at 90C overnight, the reaction mixture was diluted with ethyl acetate (40 mL), water (10 mL) was added, and the layers were separated. The aqueous layer was extracted with ethyl acetate (2 x 40 mL), and the combined organic layers were dried over sodium sulfate, filtered and concentrated. The residue was purified by flash chromatography (puriFlash, Interchim, cyclohexane/ethyl acetate 1 : 1 to 100% ethyl acetate gradient) to yield the title product as a slightly yellow solid. Yield: 304 mg (81 % of th.). HPLC (method 10): R, = 0.83 min; LC-MS (method 10): RT = 0.57 min; MS (ESIpos): m/z (%) = 1 75. 1 (100) [M+H]+. ? Iota NMR (400 MHz, 4J-DMSO): delta (ppm) = 2.15 (s, 3H), 5.22 (m, 1H), 6.30 (m, H I ). 6.73 (d, 1H), 6.91 (d, 1H), 7.69 (m, 1H), 7.91 (s, 1H).

The synthetic route of 937046-98-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; Bayer Pharma Aktiengesellschaft; KLAR, Juergen; VOEHRINGER, Verena; TELSER, Joachim; LOBELL, Mario; SUessMEIER, Frank; LI, Volkhart Min-Jian; BOeTTGER, Michael; GOLZ, Stefan; LANG, Dieter; SCHLEMMER, Karl-Heinz; SCHLANGE, Thomas; SCHALL, Andreas; FU, Wenlang; WO2013/4551; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 452-92-6, name is 5-Bromo-2,4-difluoroaniline, 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 452-92-6, COA of Formula: C6H4BrF2N

General Procedure: Methyl 2-{[4-(chlorosulfonyl)-2,3-dimethylphenyl]oxy}propanoate (7) (4 g, 13.0 mmol) was dissolved in pyridine (10 mL). After 5 min, 3-bromo-2-chloroaniline (3.22 g, 15.6 mmol) was added. The reaction was complete within a few hours. The reaction mixture was then extracted using diethyl ether. The combined organic phases were washed with 1N HCl and brine, dried over sodium sulfate, filtered, and concentrated in vacuo to afford the title compound which was used without further purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Bromo-2,4-difluoroaniline, and friends who are interested can also refer to it.

Reference:
Article; Evans, Karen A.; Shearer, Barry G.; Wisnoski, David D.; Shi, Dongchuan; Sparks, Steven M.; Sternbach, Daniel D.; Winegar, Deborah A.; Billin, Andrew N.; Britt, Christy; Way, James M.; Epperly, Andrea H.; Leesnitzer, Lisa M.; Merrihew, Raymond V.; Xu, Robert X.; Lambert, Millard H.; Jin, Jian; Bioorganic and Medicinal Chemistry Letters; vol. 21; 8; (2011); p. 2345 – 2350;,
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. 108-85-0, name is Bromocyclohexane, A new synthetic method of this compound is introduced below., COA of Formula: C6H11Br

General procedure: Na2S·3H2O (0.291 g, 2.2 mmol) was addedto a magnetically stirred solution of an alkyl halide (2 mmol) and C2Cl6 or CCl4 (1.5 mmol) in PEG-200 (2 mL) at r.t. The stirring was continued until the starting halide was completely consumed (30-150 min). Next, the reaction mixture was diluted with H2O (1 mL) and extracted with EtOAc-hexane (1:1;4 × 2 mL). The organic extracts were combined, concentrated and purified by chromatography on silica gel. The desired disulfides were produced in excellent yields (Table 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:
Article; Abbasi, Mohammad; Mohammadizadeh, Mohammad Reza; Moosavi, Hekmat; Saeedi, Narges; Synlett; vol. 26; 9; (2015); p. 1185 – 1190;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1074-24-4,Some common heterocyclic compound, 1074-24-4, name is 1,4-Dibromo-2,5-dimethylbenzene, molecular formula is C8H8Br2, 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.

1,4-dibromo-2,5-dimethylbenzene: 1H-1,2,4- triazole: potassium carbonate: copper oxide molar ratio is 2: 10: 30: 1. To a 50mL three-neck round bottom flask equipped with a magnetic stirrer, reflux condenser and thermometer was added CuO (0.0398mg,0.5mmol), potassium carbonate (2.0731g, 15mmol), 1H-1,2,4-triazole (0.345mg, 5mmol), 1,4- dibromo-2,5-dimethylbenzene (0.3360g, 1mmol ), 20mL DMF. Stirring at 100 deg.C. React for 24 hours. After completion of the reaction, the reaction solution was cooled to room temperature, filtered and the filtrate was added 100mL of water, heavy precipitate precipitation, filtration, filter cake was collected, yield 60percent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,4-Dibromo-2,5-dimethylbenzene, its application will become more common.

Reference:
Patent; Tianjin Normal University; Wang, Ying; (11 pag.)CN105669720; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 656-64-4, name is 3-Bromo-4-fluoroaniline, molecular formula is C6H5BrFN, 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. COA of Formula: C6H5BrFN

Benzoyl chloride (18.5 g, 132 mmol) was added to a solution of ammonium thiocyanate (12 g, 158 mmol) in acetone (350 mL) over 5 minutes and the mixture was refluxed for 15 minutes. 3-Bromo-4-fluoroaniline (25 g, 132 mmol) was added to the mixture at 40 and refluxing was continued for 30 minutes. The hot solution was poured over ice (400 mL) and the mixture was stirred for 5 minutes until a precipitate formed, which was collected by filtration and washed with 50% methanol in water (50 mL). To the precipitate was added a 5% sodium hydroxide solution (1000 mL) and the suspension was stirred for 2 hours at 60*0. The mixture was ai lowed to cool down to room temperature and stored at room temperature for 3 days while a precipitate formed, which was collected by filtration, washed with water and dried under reduced pressure to yield 22.2 g (67%) 1-(3-bromo-4-fluorophenyl)thiourea1 H-NMR (300 MHz, DMSO-cfe) delta = 7.34 (dd, 1 H), 7.35 (ddd, 1 H), 7.59 (br, 2H), 7.85 (dd, 1 H) 9.75 (br, 1 H) ppm.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 656-64-4, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; ROeHN, Ulrike; SCHMITT-WILLICH, Heribert; HEINRICH, Tobias; BERGER, Markus; FITZNER, Ansgar; KRAUSE, Sabine; BROCKSCHNIEDER, Damian; DYRKS, Thomas; THIELE, Andrea; MOeNNING, Ursula; BOeMER, Ulf; WO2012/7510; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 583-75-5, These common heterocyclic compound, 583-75-5, name is 4-Bromo-2-methylaniline, 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.

EXAMPLE 192 1,2-Dihydro-6-(3-nitrophenyl)-2,2,4,8-tetramethylquinoline (Compound 292, structure 86 of Scheme XXII, where R1 =R3-5 =H, R2 =nitro) 4-Bromo-2-methylaniline (5.58 g, 30 mmol) was treated with iodine (0.2 g, 0.9 mmol) and acetone (150 mL) in a sealed tube at 80 C. for 24 h to provide 6-bromo-1,2-dihydro-8-methylquinoline (Compound 85 of Scheme XXII) in 9% yield as a yellow oil (0.70g). Most of the aniline (>80%) was recovered.

The synthetic route of 583-75-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ligand Pharmaceuticals Incorporated; US5693647; (1997); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 4549-33-1, 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 4549-33-1 as follows.

General procedure: Furanchalcone or quinoline (1 mmol), potassium hydroxide(1.5 mmol, 84.2 mg) and acetonitrile (10 mL), were placedin a 25 mL flat-bottomed flask equipped with a magneticstirring bar. The mixture was stirred and heated to reflux fora period of 5 min, under microwave irradiation. Then, 1,omega-dibromoalkane (1.1 mmol) was added to the reaction mixture,which was refluxed for 30 min (200 W). The crudereaction mixture was concentrated on a rotatory evaporatorand the residue was purified by column chromatographyover silica gel eluting with hexane and a mixture of hexaneethylacetate (9:1 ratio) to obtain bromoalkyl derivatives inyields ranging between 61 and 76%. Monitoring of thereaction progress and product purification was carried outby TLC.

According to the analysis of related databases, 4549-33-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Garcia, Elisa; Coa, Juan C.; Otero, Elver; Carda, Miguel; Velez, Ivan D.; Robledo, Sara M.; Cardona, Wilson I.; Medicinal Chemistry Research; vol. 27; 2; (2018); p. 497 – 511;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 33070-32-5, 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. 33070-32-5 name is 5-Bromo-2,2-difluorobenzodioxole, 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 250 mL round bottom flask with stir bar was charged with toluene (100 mL), and the solvent was sparged with N2 for one hour. Trisodium phosphate (20.75 g, 127 mmol) was added, followed by bis(dibenzylideneacetone)palladium (0.970 g, 1.68 8 mmol). A solution of tri-tert-butylphosphine (0.683 g, 3.38 mmol) was added over 10 minutes via syringe, and the suspension was stirred for 50 minutes at 25C. 5-Bromo-2,2-difluorobenzo[dj[1,3jdioxole (10 g, 42.2 mmol) was added, and after stirring for 50 minutes at 25 C, ethyl 2-cyanoacetate (9.55 g, 84 mmol) was added over 5 minutes, followed by the addition of 1.5 mL of water. The reaction was heated at 75 C for 12 hours. Three additional vials were set up as described above. After completion of the reaction, all four reaction mixtures were combined. The reaction was cooled to 25 C and filtered over diatomaceous earth. The filtrate was concentrated, and the residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate = 5/1) to provide the title compound (24.5 g, 48.5 % yield). ?H NMR (400 MHz, DMSO-d6) 6 ppm 1.15 – 1.23 (m, 3 H) 4.13 – 4.29 (m, 2 H) 7.30 (dd, J=8.38, 1.76 Hz, 1 H) 7.46 – 7.55 (m, 2 H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Bromo-2,2-difluorobenzodioxole, and friends who are interested can also refer to it.

Reference:
Patent; ABBVIE S.A.R.L.; GALAPAGOS NV; CHAN, Vincent S.; KYM, Philip R.; SHEKHAR, Shashank; WANG, Xueqing; (89 pag.)WO2018/116185; (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. 630-17-1, name is 1-Bromo-2,2-dimethylpropane, A new synthetic method of this compound is introduced below., HPLC of Formula: C5H11Br

A mixture of 4,5,6,7-tetrahydro-1H-benzo[d]imidazole (5.00 g, 40.9 mmol),90% KOH (3.74 g, 60 mmol) and DMSO (70 mL) was stirred under argon and heated at 40 C for 2 h. After cooling to 10 C, neopentyl bromide (5.5 mL, 44 mmol) was added in one portion, and the resulting mixture was stirred and heated at 40 C for 4 days. The reaction mixture was poured into ice/water (800 mL), treated with 5 NNaOH (200 mL), and extracted with DCM (2 x 400 mL). The extract was washed with water (200 mL), dried over Na2SO4, and the solvent was removed under reduced pressure to give a residue. Column chromatography of the residue (silica gel, ethyl acetate/methanol, 95:5) afforded pure 1-neopentyl-4,5,6,7-tetrahydro-1H- benzo[d]imidazole (4.72 g, 60% yield).

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; NITTO DENKO CORPORATION; STANISLAW, Rachwal; HU, Yufen; ZHANG, Hongxi; WANG, Peng; (42 pag.)WO2018/191238; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 2695-48-9, name is 8-Bromo-1-octene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 8-Bromo-1-octene

15.(1) Synthesis of p-(7-octenyloxy)benzoic acid 9.4 g of 8-bromo-1-octene, 9.0 g of ethyl p-hydroxybenzoate, and 7.6 g of potassium carbonate were refluxed in ethanol for 10 hours. Added thereto was an aqueous solution containing 2.4 g of sodium hydroxide, and reflux was further continued for 10 hours. After conclusion of the reaction, the reaction solution was diluted with water, and the pH of the diluted solution was lowered to 2 by dropping hydrochloric acid thereto. The generated precipitate was collected, and was then washed with water sufficiently and dried, to obtain 10.8 g of the objective ether compound. (Yield: 89 %)

The synthetic route of 2695-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IDEMITSU KOSAN COMPANY LIMITED; EP355772; (1991); A3;,
Bromide – Wikipedia,
bromide – Wiktionary