Month: March 2021

Adding a certain compound to certain chemical reactions, such as: 937046-98-5, name is 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine, 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 937046-98-5, Application In Synthesis of 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine

To a solution of 2-1 (3.85 g, 18.1 mmol, WO 2007/64931, published June 7, 2007) in anhydrous DMF (30 mL) was added NaH (1.08 g, 27.1 mmol) at 0 C. The reaction was stirred under N2 for 0.5 h. MMTrCl (6.14 g, 19.9 mmol) was added. The mixture was stirred at RT for 2 h. Water was added to quench the reaction. The mixture was extracted with EA (3 X 100 mL). The organic phase was combined and then dried over Na2SO4. After filtration, the solution was concentrated in vacuo to give a residue which was further purified by column chromatograph (PE:EA = 20: 1) to give 2-2 (3.8 g, 45%) as a white solid. ESI-LCMS: m/z 485.2 [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, 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ALIOS BIOPHARMA, INC.; BEIGELMAN, Leonid; WANG, Guangyi; ZHONG, Minghong; (249 pag.)WO2017/156262; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 103977-79-3, 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 103977-79-3 as follows.

A mixture of 106 2,2-dimethyl-1,3-dioxane-4,6-dione (7.62 g, 52.88 mmol) in 107 trimethoxymethane (26.3 mL, 240.38 mmol) was heated at 85 C. and stirred for 1.5 h. 498 3-Bromo-2,4-difluoroaniline (10 g, 48.08 mmol) in 33 ethanol (42.4 mL) was added and the reaction mixture was stirred at 85 C. for 3 h. The mixture was cooled with the resulting solid was filtered and washed with IPA (2¡Á50 mL) and diethyl ether (4¡Á50 mL). The solid was dried under vacuum overnight to afford 499 5-[(3-bromo-2,4-difluoroanilino)methylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione (14.62 g, 84%) as a beige solid; 1H NMR (400 MHz, DMSO, 30 C.) 1.69 (6H, s), 7.33-7.43 (1H, m), 7.86-7.97 (1H, m), 8.56-8.64 (1H, m), 11.24 (1H, s); m/z: ES+ [M+H]+ 362.0.

According to the analysis of related databases, 103977-79-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; Kettle, Jason Grant; Bagal, Sharanjeet; Robb, Graeme Richard; Smith, James Michael; Goldberg, Frederick Woolf; Cassar, Doyle Joseph; Feron, James Lyman; US2019/177338; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 201138-91-2, A common heterocyclic compound, 201138-91-2, name is 4,6-Dibromodibenzo[b,d]furan, molecular formula is C12H6Br2O, 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.

10.43 g (32 mmol) of B-(9-phenyl-9H-carbazole-3-yl)boronic acid, 8.9 g (31.6 mmol) of 4,6-dibromodibenzofuran and 31 mL (63 mmol) of Na2CO3 (2 M solution) was then suspended in 120 mL of toluene and 120 mL ethanol. To this suspension, it was added 0.73 g (0.63 mmol) of Pd(PPh3)4 and heat the reaction mixture for 16 hours under reflux. After cooling, remove the organic phase, after filtration, washed three times with 200 mL through silica gel, and concentrated until dry. Recrystallization of the residue from toluene. The yield for the 73% of theory, 11.4 g

The synthetic route of 201138-91-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck patent GmbH; Hussain, Farham Amir; Martinopa, Irina; Yachi, Anya; Avelluley, Thomas; Kuriba, JonasFallentine; (111 pag.)KR2016/38006; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 10485-09-3, name is 2-Bromoindene, 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 10485-09-3, Quality Control of 2-Bromoindene

n a fully dried, argon purged 100 mL reactor,JP-A-2012-206997 2. 4-g 2- (5-methyl-2-furyl) -1-indene synthesized by the method described in the publicationCharge (15.0 mmol) and 20 mL of tetrahydrofuran,n-Butyllithium solution 9.70 mL(Hexane solution, 1.55 M, 15.0 mmol) is added,Stir at room temperature for 2 hours. This reaction solution is9.00 mL (75.3 mmol) of dimethylsilyl dichloride in 10 mL of n-hexane diluted solutionAdd slowly while cooling at -78 C,Stirring was continued for 20 hours while returning to room temperature.After the solvent of the reaction solution and unreacted dimethylsilyl dichloride were distilled off, 20 mL of tetrahydrofuran and 1.50 mL (16.0 mmol) of 1,3-dimethyl-2-imidazolidinone were added to the residue.In a fully dried, argon purged 200 mL reactor, 1.45 g (59.8 mmol) of magnesium pieces are charged,Stir vigorously for 30 minutes while heating under reduced pressure.After cooling to room temperature, attach a reflux condenser,A piece of iodine and 10 mL of tetrahydrofuran were charged and stirred.After dropwise addition of 1.0 mL of a dilute solution of 2.93 g (15.0 mmol) of 2-bromoindene in 10 mL of tetrahydrofuran,Heat to reflux until the iodine color disappears in the dryer,After the reaction starts, the remaining droplets areAfter completion of the dropwise addition, the mixture was stirred at room temperature for 2 hours.This solution isAdd dropwise to the previous reaction residue dilution solution cooled to -78 C,Stirring was continued for 19 hours while slowly warming to room temperature.Add saturated aqueous ammonium chloride solution,The soluble fraction is extracted with n-hexane and the obtained fraction is saturated.Washed with Japanese salt water and dried over anhydrous magnesium sulfate.After filtering the magnesium sulfate,The residue obtained by distilling off the filtrate is purified by silica gel column chromatography,Target object shown by the following formula (A-3L)(Hereafter referred to as the compound (A-3L))Was obtained as an isomer mixture of 2.55 g (46% 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, 2-Bromoindene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Mitsui Chemicals, Inc.; Prime Polymer Co., Ltd.; Tanaka, Yoichi; Harada, Yoichi; Tamura, Naoya; Hato, Ikki; Tsuchiya, Hiroko; (55 pag.)JP2019/59724; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 58971-11-2, The chemical industry reduces the impact on the environment during synthesis 58971-11-2, name is 3-Bromophenethylamine, I believe this compound will play a more active role in future production and life.

To a solution of methanesulfonyl chloride(1.60 mmol, 0.12 mL, 1.0 equiv) in ethanol (3 mL), 2-(3-bromophenyl)ethan-1-amine (3.20 mmol, 639mg, 2.0 equiv) was added and the mixture was stirred at room temperature. The reaction wasmonitored by TLC. After completion the solvent was removed under reduced pressure and theremaining solid dissolved in a small amount of water. The solution was applied to a C18 precolumnbefore purification on a 60 g C18 column with a gradient of acetonitrile in water (10-80%). The titlecompound (1.07 mmol, 295 mg, 66%) was obtained as a white solid.

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, 3-Bromophenethylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Akhter, Sundus; Lund, Bjarte Aarmo; Ismael, Aya; Langer, Manuel; Isaksson, Johan; Christopeit, Tony; Leiros, Hanna-Kirsti S.; Bayer, Annette; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 634 – 648;,
Bromide – Wikipedia,
bromide – Wiktionary

348-57-2, name is 1-Bromo-2,4-difluorobenzene, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C6H3BrF2

EXAMPLE 16 Preparation of 4-(2,4-difluorophenyl)-anisole from 4-methoxyphenylmagnesiumbromide and palladium acetate/triphenylphosphine (0.1percent) A suspension of magnesium turnings (13.5 g; 555 mmoles–Janssen) in tetrahydrofuran (132.9 g) was heated at 65¡ã C. under stirring and under nitrogen. Then, iodine (0.35 g) and, after 30 minutes, 4-bromoanisole (102.65 g; 549 mmoles), in 1 hour, were added to the reaction mixture. At the end of the addition, the reaction mixture was kept at 75¡ã C. for 1 hour and, then, decanted obtaining a solution of 4-methoxyphenylmagnesiumbromide (solution A). A mixture of 1-bromo-2,4-difluorobenzene (100 g; 518 mmoles), palladium acetate (0.11644 g; 0.519 mmoles–Janssen) and triphenylphosphine (0.54356 g; 2.07 mmoles–Fluka) was de-aerated by vacuum/nitrogen at 25¡ã C. The mixture was heated at 85¡ã C., kept under stirring for 15 minutes and, then, solution A was added in 6 hours. At the end of the addition, the reaction mixture was kept at 85¡ã C. for 30 minutes. After cooling at 60¡ã C., a solution of 37percent hydrochloric acid (17.5 ml) in water (88 ml) was added in 20 minutes. The mixture was cooled at 40¡ã C. and the phases were separated. The solvent of the organic phase was evaporated under reduced pressure obtaining the desired compound (113 g; HPLC titre 93.71percent; 93percent yield).

The synthetic route of 348-57-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zambon Group S.p.A.; US5312975; (1994); A;,
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. 3972-65-4, name is 1-Bromo-4-(tert-butyl)benzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-(tert-butyl)benzene

A typical procedure of the electroreductive coupling of aryl bromide1 with catalytic amounts of [OctV2+][Tf2N]2 and Pd species isas follows. Into an undivided cell fitted with a Zn anode(1.5 1 cm2) and a Pt cathode (1.5 1 cm2) was added a DMF(3 mL) solution of 4-bromopropiophenone (1a, 0.25 mmol),[Bu4N+][Tf2N] (0.3 mmol), [OctV2+][Tf2N]2 (0.075 mmol,30 mol %), and PdCl2(PPh3)2 (0.0125 mmol, 5 mol %). The wholemixture was electrolyzed at 60 C under constant current(10 mA) conditions until 2 F/mol-1a of electricity was passed.The reaction mixture was poured into 5% aq HCl and extractedwith AcOEt. Purification by column chromatography (SiO2, toluene/AcOEt = 10/1) afforded 4,40-dipropanoylbiphenyl (2a) in 94%yield

The synthetic route of 3972-65-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kuroboshi, Manabu; Shiba, Takuya; Tanaka, Hideo; Tetrahedron Letters; vol. 54; 28; (2013); p. 3666 – 3668;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 6274-57-3, These common heterocyclic compound, 6274-57-3, name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, 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.

nBuLi (2.5 M in hexanes, 2.15 mL, 5.37 mmol) was added dropwise to a solution of 1-(4- bromophenyl)-N,N-dimethylmethanamine (1.0 g, 4.67 mmol) in THF (10 mL) at -78 C and the reaction was stirred for 15 min. SO2 was bubbled through the solution for 5 min, then the reaction was warmed to RT. After 2 h, the reaction was concentrated to almost dryness then triturated with MTBE (40 mL) and the solid was filtered to afford the title compound (0.8 g, 71% yield) as a yellow solid.1H NMR (DMSO-d6) d 7.45 (d, J = 7.7 Hz, 2H), 7.30 (d, J = 7.6 Hz, 2H), 3.62 (s, 2H), 2.20 (s, 6H).

The synthetic route of 6274-57-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INFLAZOME LIMITED; MILLER, David; MACLEOD, Angus; THOM, Stephen; MCPHERSON, Christopher G.; ALANINE, Thomas; CARRILLO ARREGUI, Jokin; CIANA, Claire-Lise; SHANNON, Jonathan; VAN WILTENBURG, Jimmy; DEN HARTOG, Jacobus Antonius Joseph; (603 pag.)WO2019/211463; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1003-99-2, 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. 1003-99-2, name is 2-Bromo-5-fluoroaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2-Bromo-5-fluoro-aniline (2.50 g, 95 mass percent article, 12.5 mmol), m-nitrobenzenesulfonic acid (1.33 g, 6.53 mmol), 10.0 mL of 85 wtpercent aqueous phosphoric acid solution and ferrous sulfate heptahydrate (34.8 mg, 0.125 mmol) were placed in a 100 mL three-neck flask equipped with a magnetic stirrer, a reflux condenser, a thermometer and a dropping funnel and the mixture was heated to 80¡ãC in an oil bath. Subsequently, 2.32 g of methacrolein (98 mass percent article, 32.5 mmol) was added dropwise thereto through the dropping funnel for 1 hour. After completion of the dropwise addition, the mixture was heated and stirred at 100¡ãC for 2 hours. Then, the reaction mixture was poured into water and neutralized to pH 7 by ammonia water. The neutralized liquid was extracted with dichloromethane and then, dichloromethane was removed under reduced pressure. The resulting crude reaction product was purified by column chromatography (Hexane/AcOEt=100/0->1/1) using silica gel, followed by drying under reduced pressure to give 730 mg of 8-bromo-5-fluoro-3-methyl-quinoline as a yellow white solid (yield: 24.3percent). 1H-NMR (300 MHz, CDCl3) delta: 8.93 (d, 1H), 8.22-8.19 (m, 1H), 7.93-7.87 (m, 1H), 7.13-7.07 (m, 1H), 2.59 (s, 3H) [MS] EI (m/z): 240 (M+), CI (m/z): 241 (MH+)

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

Reference:
Patent; Ube Industries, Ltd.; EP1847545; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 2044-08-8, name is 1-Bromocyclohex-1-ene, 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 2044-08-8, Recommanded Product: 1-Bromocyclohex-1-ene

Under nitrogen protection, 20 g (0.12 mol) of 1-bromo-1-cyclohexene and 34.7 g (0.14 mol) of pinacol borate were added to the three-necked flask.2.0 g (6 mol%) of triphenylphosphine,2.6 g (3 mol%) of trans-bis(triphenylphosphine)palladium(II) dichloride,Potassium phenolate 24.6 g (0.19 mol) and anhydrous toluene 250 mL.After nitrogen substitution, the reaction was stirred at 50 C for 5 hours.The system was then cooled to room temperature and quenched with water.The reaction mixture was extracted with a benzene solvent and brine.The organic phase was dried over anhydrous magnesium sulfate.The dried mixture was filtered and concentrated under reduced pressure.It can be purified by silica gel column or distillation to obtain 21.9 g (yield: 85%)Cyclohexene-1-boronic acid pinacol ester.

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-Bromocyclohex-1-ene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Yurui (Shanghai) Chemical Co., Ltd.; Zheng Xianzhe; (51 pag.)CN109206457; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary