Month: August 2021

Adding a certain compound to certain chemical reactions, such as: 51437-00-4, name is 4-Bromo-1-fluoro-2-methylbenzene, 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 51437-00-4, Recommanded Product: 51437-00-4

Example 96 Preparation of 3-Methyl-2-(1H-1,2,4-triazol-1-yl)-5-vinylbenzonitrile (DI70) Step 1. 5-Bromo-2-fluoro-3-methylbenzaldehyde To a stirred solution of di-isopropyl amine (4.01 g, 39.88 mmol) in THF (20 mL) was added n-butyl lithium (1.6 M in hexane) (19.9 mL, 31.91 mmol) at -78 C. slowly dropwise over the period of 10 min, the reaction mixture was stirred at -78 C. for 30 min. A solution of 4-bromo-1-fluoro-2-methylbenzene (5.0 g, 26.6 mmol) in THF (30.0 mL) was added at -78 C., and the reaction mixture was stirred for 1 h at the same temperature. DMF (5.0 mL) was added and stirred at -78 C. for another 30 min. The reaction was monitored by TLC; then the reaction mixture was quenched with 1N HCl solution (aq) at 0 C. The aqueous layer was extracted with diethyl ether, washed with water and saturated brine solution. The combined organic layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure to obtain the crude compound purified by flash column chromatography (SiO2, 100-200 mesh; eluting with 5% ethyl acetate/pet ether) to afford the title compound as a white solid (3.6 g, 64%); mp 48-50 C.: 1H NMR (400 MHz, CDCl3) delta 8.33 (s, 1H), 8.22 (s, 1H), 7.67 (s, 1H), 7.60 (s, 1H), 6.75 (dd, J=17.6, 10.8 Hz, 1H), 5.92 (dd, J=17.6, 10.8 Hz, 1H), 5.52 (d, J=17.6 Hz, 1H), 2.21 (s, 3H); ESIMS m/z 211.35 ([M-H]-).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Dow AgroSciences LLC; Lo, William C.; Hunter, James E.; Watson, Gerald B.; Patny, Akshay; Iyer, Pravin S.; Boruwa, Joshodeep; US9211280; (2015); B2;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 61613-22-7, These common heterocyclic compound, 61613-22-7, name is 2-Bromo-N-phenylaniline, 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.

33 g (145 mmol) of di-tert-butyl dicarbonate first fill in 600 mL of toluene. To this solution 27g (110 mmol) of (2-bromophenyl)phenylamine and 1.3 g (11 mmol) of 4-dimethylaminopyridine, The mixture is boiled under reflux for 40 h. Subsequently 200mL of water was added to the reaction and separating the organic phase, the solvent was removed under reduced pressure. The residue was then recrystallized from hot hexane. Yield: 36 g (103 mmol), 95%.

Statistics shows that 2-Bromo-N-phenylaniline is playing an increasingly important role. we look forward to future research findings about 61613-22-7.

Reference:
Patent; Merck Patent GMBH; Farrahm, Amir Hossain; Flume, Christoph; Everille, Thomas; Yatsi, Anya; Montenegra, Elvira; Krober, Jonas Valentine; Rinke, Roophen; (59 pag.)KR2016/27155; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, 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 314084-61-2, name: 2-Bromo-1,3-diethyl-5-methylbenzene

Under a nitrogen atmosphere and at normal pressure, 14 g of malonic acid dinitrile dissolved in 7 ml of 1-methyl-2-pyrrolidone are added dropwise in the course of 30 minutes, at from 20 to 25C, to a mechanically stirred mixture of 64 g of sodium carbonate in 200 mi of 1-methyl-2-pyrrolidone. The reaction mixture is heated to 100C and 45.5 g of 2-bromo- 1, 3-diethyl-5-methylbenzene are added, after which the mixture is heated to 120C. At that temperature, a mixture of 0.26 g of TRIPHENYLPHOSPHINE, 0.21 g of a commercially available palladium (LI) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.071 g of PALLADIUM (II) CHLORIDE in 0.142 g of concentrated hydrochloric acid) and 19.5 g of 1-methyl-2-pyrrolidone is added. The reaction mixture is stirred for from 2 to 3 hours at from 125 to 140C. A gas chromatogram of a sample (1 ml of reaction mixture partitioned between 2 ML of 1 N hydrochloric acid and 2 ml of tert-butyl methyl ether) shows that the product (2-(2, 6-DIETHYL-4-METHYLPHENYL) MALONIC acid dinitrile) has not formed.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; WO2004/50607; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 57951-72-1, name is 1-Bromo-2-cyclopropylethyne, 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 57951-72-1, Formula: C5H5Br

General procedure: Dissolved aryl halide (1.0 equiv) in dry DMF and subjected to degassing with a gaseous mixture of (H2+ N2) balloon for three times. Added PdCl2(PPh3)2(10 mol %) followed by Cul (8 mol%) at r.t. Added terminal alkyne (1.0 equiv. followed by TEA. The reaction mixture stirred at 50 C or 90 C. After cooling to room temperature, the resulting solution was subjected to rotary evaporation and partitioned between EtOAc and D.I. water. Aqueous layer was extracted with EtOAc 20 mL (3x). Combined organic layers were given water, brine washes and dried over anhydrous Na2S04. After evaporation of the solvent, column chromatography on silica gel afforded the desired product.

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-2-cyclopropylethyne, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THORPE, Steven Brandon; SANTOS, Webster L.; LYNCH, Kevin R.; (375 pag.)WO2017/172989; (2017); 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. 112734-22-2, name is (4-Bromo-2-fluorophenyl)methanamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C7H7BrFN

solution of [(4-bromo-2-fluorophenyl)methyl]amine (2.Og, 9.8mmol) and triethylamine (2.73ml, 19.6mmol) in dimethylformamide (20ml) was treated with 3- chloropropanesulfonyl chloride (1.74g, 9.8mmole) dropwise over 10 minutes with stirring under argon. This mixture was stirred for 30 minutes before being treated with sodium hydride (60% suspension in mineral oil, 1.176g, 29.4mmol) portionwise and the reaction mixture stirred at room temperature for 16 hours. The reaction mixture was partitioned between water and dichloromethane. The organic layer was dried over sodium sulphate and evaporated under reduced pressure. Sample was then purified by column chromatography on silica using 10 to 90% ethyl acetate in n-pentane to afford the title compound as an oil (1.7g, 55%).LC/MS (ES): Found 308 & 310 (ES+), retention time 2.73mins. Ci0H11 BrFNO2S requires 307 & 309.1H-NMR (400MHz, CDCI3): 2.34 (2H, m), 3.19 (4H, m), 4.20 (2H, d, J=I Hz), 7.22-7.35 (3H, m).

The synthetic route of 112734-22-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2008/110566; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 626-39-1, name is 1,3,5-Tribromobenzene, 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. Formula: C6H3Br3

Under a nitrogen atmosphere, 250ml three-necked flask 1,3,5-bromobenzene (15.74g, 50mmol), United pinacolato ester (41.9g, 0.165mol, TCI), potassium acetate (48.58g, 0.495mol), 1,1′- bis (diphenylphosphino) ferrocene palladium dichloride (4.08g, 5mmol) and dimethylformamide (300ml), 85 The reaction mixture was stirred under heating 24h.After completion of the reaction naturally cooled, the reaction solution was extracted with ethyl acetate, washed with saturated brine three times, the resulting organic layer was dried over anhydrous magnesium sulfate.Filtration, the resulting filtrate was removed under reduced pressure to remove the solvent.Separated by column chromatography, the mobile phase was chloroform.After the spin-dry vacuum dried to give a white powder 16.25g, yield 71.3%.

The synthetic route of 1,3,5-Tribromobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; South China University of Technology; Su, Shijian; Chen, Dongcheng; (24 pag.)CN103396355; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 2635-13-4,Some common heterocyclic compound, 2635-13-4, name is 5-Bromobenzo[d][1,3]dioxole, molecular formula is C7H5BrO2, 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 3 Alternative syntheses of (S)-alpha-methyl-1,3 benzodioxole-5-ethanol 3.47 grams of 4-bromo-1,2(methylenedioxy)benzene were dissolved in 100 ml of tetrahydrofuran at -78 C., 13.9 ml of 1.3M sec-butyllithium in cyclohexane was then added to consume the aryl halide in less than 30 minutes. 1.00 grams of (S)-(-)-propylene oxide in 2 ml THF was added by syringe and the solution stirred for 45 minutes. The solution was then warmed to 23 C. for 16 hours. The reaction mixture was poured into 3M ammonium chloride solution and the product isolated by extraction with ethyl acetate. The combined extracts were dried over magnesium sulfate filtered through florisil and concentrated by rotary evaporation. The residual oil was purified by silica gel chromatography and eluted with a 50:50 mixture of hexane and diethyl ether to yield 1.40 g (45%) of the subtitled intermediate. Pchem: [alpha]365 +117.2 (c 1.0, CHCl3) TLC Rf =0.26 (50:50 hexane:ether); IR (CHCl3) 3598, 3012, 2973, 2887, 1490, 1249, 1041cm-1; 13 C NMR (CDCl3) d 147.75, 146.19, 132.26, 122.27, 109.68, 108.30; mass spectrum, m/z (FD, M+) 180; Anal. Calcd. for C10 H12 O3: C, 66.65; H, 6.71. Found: C, 66.42; H, 6.66.

The synthetic route of 2635-13-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Eli Lilly and Company; US5665878; (1997); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 1003-99-2, name is 2-Bromo-5-fluoroaniline, 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 1003-99-2, Safety of 2-Bromo-5-fluoroaniline

N-(2-Bromo-5-fluorophenyl)pivalamide. Trimethylacetyl chloride (4.2 mL, 34.1 mL) was fast dropwise added to a solution of 2-bromo-5-fluorobenzenamine (4.31 g, 22.7 mmol) in CH2Cl2 (50 mL) at room temperature, followed by the addition of DIEA (7.9 mL, 45.4 mmol). The resulting mixture was stirred at room temperature for 2 hrs, and then partitioned between HCl (1N, 200 mL) and EtOAc (250 mL). After separation, the organic phase was washed with brine (50 mL), dried on MgSO4, concentrated on rotary vacuum, and purified on flash chromatography eluting with 2040percent EtOAc/hexanes (1200 mL) to afford the expected product, as a colorless oil (6.07 g, 98percent yield); 1H NMR (400 MHz, CDCl3) delta ppm 1.33 (s, 9H), 6.69 (ddd, J=8.81, 7.55, 3.02 Hz, 1H), 7.45 (dd, J=8.81, 5.79 Hz, 1H), 8.04 (s, 1H), 8.28 (dd, J=11.08, 3.02 Hz, 1H); Mass spec. 274.04 (MH+), Calc. for C11H13BrFNO 273.02

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; Chaturvedula, Prasad V.; Mercer, Stephen E.; Fang, Haiquan; US2006/94707; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 4117-09-3,Some common heterocyclic compound, 4117-09-3, name is 7-Bromo-1-heptene, molecular formula is C7H13Br, 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.

In a round-bottom flask, tetrabutylammonium iodide(0.02 eq.) and potassium phthalimide (2.0 eq.) were suspended in acetonitrile. 17 (1.0 eq.) was addeddropwise and the resulting mixture was heated up to 80C for exactly 24 hours. Once the mixturereached room temperature, it was diluted with diethyl ether and passed through a celite plug. Thefiltrate was concentrated in vacuo and the yellow residue was purified by column chromatography(hexane/ethyl acetate 95/5) giving the desired product as a white solid (83% yield).

The synthetic route of 4117-09-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Czescik, Joanna; Zamolo, Susanna; Darbre, Tamis; Mancin, Fabrizio; Scrimin, Paolo; Molecules; vol. 24; 15; (2019);,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 24358-62-1, 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. 24358-62-1, name is 1-(4-Bromophenyl)ethylamine, This compound has unique chemical properties. The synthetic route is as follows.

A solution of 4-bromo-alpha-methylbenzylamine (1.5 g, 7.7 mmol), 3-pyridinecarboxaldehyde (0.8 g, 7.5 mmol), and sodium triacetoxyborohydride (2.25 g, 10.5 mmol) in 60 ml of 1,2-dichloroethane was stirred at room temperature for 18 h. The solution was diluted with dichloromethane and washed twice with a saturated sodium bicarbonate solution, once with water, and once with brine. The organic layer was separated, dried over sodium sulfate, filtered, and concentrated in vacuo to afford the title compound. 1H NMR: 8.70 (m,2H), 7.85 (m,1H), 7.67 (d,2H,J=8 Hz), 7.45 (d,2H,J=8 Hz), 7.43 (m,1H), 3.95 (q,1H,J=8 Hz), 3.83 (q,ABX,2H), 1.57 (d,3H,J=8 Hz). MS calcd. 291.2; MS (M+1) 292.1.

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

Reference:
Patent; Coleman, Darrell Stephen; Jagdmann, Gunnar Erik; Johnson, Kirk Willis; Johnson, Michael Parvin; Large, Thomas Hallett; Monn, James Allen; Schoepp, Darryle Darwin; Barda, David Anthony; Britton, Thomas Charles; Dressman, Bruce Anthony; Henry, Steven Scott; Hornback, William Joseph; Tizzano, Joseph Patrick; Fichtner, Michael William; US2004/6114; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary