Extracurricular laboratory: Synthetic route of 698-00-0

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-N,N-dimethylaniline, other downstream synthetic routes, hurry up and to see.

Related Products of 698-00-0, 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. 698-00-0, name is 2-Bromo-N,N-dimethylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a stirred solution of N,N-dimethylanilines (1, 1.0 mmol) and 2,3-dihydrofuran (2, 10 mmol) in MeCN(20 ml), Co(ClO4)2 (10 mol%) was added. The reactions were performed at 50 C under oxygen atmosphere(O2 balloon) and completed in 48 hours. The products 3 were isolated by flash column chromatographic separation (acetone/petroleum ether = 1:40 to 1:30).

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-N,N-dimethylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Huo, Congde; Chen, Fengjuan; Quan, Zhengjun; Dong, Jie; Wang, Yajun; Tetrahedron Letters; vol. 57; 46; (2016); p. 5127 – 5131;,
Bromide – Wikipedia,
bromide – Wiktionary

Share a compound : 74586-53-1

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

Adding a certain compound to certain chemical reactions, such as: 74586-53-1, name is 3-Bromo-5-methylaniline, 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 74586-53-1, Quality Control of 3-Bromo-5-methylaniline

[0251] 3-Bromo-5-methylaniline (372.2 mg, 2.0 mmol) was dissolved in aqueous 1 N hydrochloric acid (160 mL), and acrolein diethylacetal (762 mu^, 5.0 mmol) was added. The reaction mixture was heated to reflux for 24 hours. After cooling to room temperature, the dark brown solution was neutralized with solid potassium carbonate and extracted with dichloromethane (3 x 150 mL). Combined organic layers were washed with brine (1 x 150 mL), dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified on silica gel using a mixture of dichloromethane and methanol (100:0 to 90: 10 gradient) as eluent. The product was obtained as brown oil as a mixture of isomers Int-2 and Int-2A (1.5: 1) in 35% yield. Major isomer: ‘H- MR (500 MHz, CDC13): delta 8.88 (dd, J = 4.2, 1.3 Hz, 1H), 8.46 (d, J = 8.5 Hz, 1H), 7.85 (s, 1H), 7.68 (s, 1H), 7.42 (dd, J= 8.5, 4.2 Hz, 1H), 2.65 (s, 3H); Minor isomer: 1H-NMR (500 MHz, CDC13): delta 8.90 (dd, J = 4.1, 1.4 Hz, 1H), 8.27 (d, J = 8.5 Hz, 1H), 8.14 (s, 1H), 7.48 (s, 1H), 7.42 (dd, J = 8.5, 4.2 Hz, 1H), 2.54 (s, 3H).

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

Reference:
Patent; ACTAVALON, INC.; DNEPROVSKAIA, Elena, V.; HOLZWARTH, Michael, S.; RYCHNOVSKY, Scott, D.; (184 pag.)WO2018/85348; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Sources of common compounds: 656-64-4

The synthetic route of 3-Bromo-4-fluoroaniline has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 656-64-4, name is 3-Bromo-4-fluoroaniline, 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. Recommanded Product: 3-Bromo-4-fluoroaniline

General procedure: To a solution of 4-chloro-2-methyl-6-nitroquinoline 12 (2.67g, 12.0mmol) and aniline 13b (1.34g, 14.4mmol) in 30mL of isopropanol (IPA) was added HCl (2 drops) at room temperature. The reaction mixture was then heated at reflux temperature for 3h. Resulting solution was cooled to room temperature. Solid separated was collected by filtration and washed with IPA. The crude product obtained was crystallized from EtOH/CH2C2 to give 14b, 1.91g (57%).

The synthetic route of 3-Bromo-4-fluoroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Marvania, Bhavin; Kakadiya, Rajesh; Christian, Wilson; Chen, Tai-Lin; Wu, Ming-Hsi; Suman, Sharda; Tala, Kiran; Lee, Te-Chang; Shah, Anamik; Su, Tsann-Long; European Journal of Medicinal Chemistry; vol. 83; (2014); p. 695 – 708;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 80058-84-0

The synthetic route of 80058-84-0 has been constantly updated, and we look forward to future research findings.

Reference of 80058-84-0, A common heterocyclic compound, 80058-84-0, name is 4-Bromo-2,6-diisopropylaniline, molecular formula is C12H18BrN, 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.

With stirring, 21 g (0.15 mol) of potassium carbonate are initially added to 141 g (1.5 mol) of phenol in 500 g of toluene, followed by the addition of 168 g (1.5 mol) of a 50percent aqueous solution of potassium hydroxide. The entire water of reaction is then separated under reflux, and then ca. 400 g of toluene are removed by distillation. The residue is dissolved in 700 g of dimethyl formamide. After addition of 6 g (0.05 mol) of copper carbonate, solvent is distilled off until the temperature of the reaction mixture is 140¡ã C. Then 256 g (1 mol) of 4-bromo-2,6-diisopropylaniline are added at 140¡ã C. and the mixture is kept for 10 hours at 140¡ã C. The dimethyl formamide is then removed by vacuum distillation, the residue is extracted with water, and the product is taken up in toluene. After stripping off the toluene, the crude product is purified by vacuum distillation, giving 215 g (80percent of theory) of 4-phenoxy-2,6-diisopropylaniline with a boiling point of 142¡ã-145¡ã C./0.04 mbar and a melting point of 69¡ã-71¡ã C., in the form of a bright red product.

The synthetic route of 80058-84-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ciba-Geigy Corporation; US4997967; (1991); A;,
Bromide – Wikipedia,
bromide – Wiktionary

New downstream synthetic route of 24358-62-1

According to the analysis of related databases, 24358-62-1, the application of this compound in the production field has become more and more popular.

Synthetic Route of 24358-62-1, 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 24358-62-1 as follows.

tert-Butyl 1-(4-bromophenyl)ethylcarbamate 1-(4-Bromophenyl)ethanamine (3.58 ml, 25 mmol) and Et3N (4.39 ml, 31.25 mmol) was dissolved in CH2Cl2 and cooled to 0 C. To this was added (Boc)2O (6.0 g, 27.5 mmol) and the resulting solution was stirred 5 minutes at 0 C. for 5 and then 3 h at room temperature. The reaction was washed with HCl (50 ml, 1M) followed by NaHCO3 (sat) (2*50 ml). The organic phase was dried over MgSO4, filtered and evaporated. The residue was purified by precipitation from MeOH/H2O (10:1) to give 6.35 g (85%) of the title compound as a white powder. 1H NMR (CDCl3) delta 7.45 (d, 2H), 7.18 (d, 2H), 4.83-4.70 (br, 2H), 1.46-1.32 (br, 12H).

According to the analysis of related databases, 24358-62-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; RESPIRATORIUS AB; US2012/40942; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Analyzing the synthesis route of 4101-68-2

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

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. 4101-68-2, name is 1,10-Dibromodecan, A new synthetic method of this compound is introduced below., Recommanded Product: 4101-68-2

Under nitrogen atmosphere, 1.23 g of compound 3, 2.97 g of 1,10-dibromodecane, 0.43 g of potassium hydroxide and 0.16 g Tetrabutylammonium bromide was added to a mixture of 10 ml of methylene chloride and 6.5 ml of water. After stirring at room temperature for 24 hours,Ml of water, washed once with 15 ml of saturated brine, the organic layer was separated, and dried over anhydrous sodium sulfate to remove water After which the solvent was removed on a rotary evaporator and purified using 200-300 mesh silica gel column chromatography (eluent ethyl acetate / petroleum ether volume 1: 30-1: 20) to give 1.41 g of the compound 4 as a colorless solid in a yield of 89%

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; Dai, Shengping; Yang, Liu; Liao, Peihai; Wang, Guixia; (8 pag.)CN106117227; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Discovery of 18087-73-5

Statistics shows that 3-Bromoimidazo[1,2-b]pyridazine is playing an increasingly important role. we look forward to future research findings about 18087-73-5.

Reference of 18087-73-5, These common heterocyclic compound, 18087-73-5, name is 3-Bromoimidazo[1,2-b]pyridazine, 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.

Tetrakis(triphenylphosphine)palladium(0) (64 mg, 55 pmol) and sodium carbonate (118 mg, 1.11 mmol) were added to a solution of 3-bromoimidazo[1,2-b]pyridazine (110 mg, 0.555 mmol) and C7 (295 mg, 0.610 mmol) in 1,4-dioxane (5 mL) and water (1 mL). The reaction mixture was degassed and purged with nitrogen several times, then placed in a sealed tube and heated at 120 C in a microwave reactor for 30 minutes. The reaction mixture was diluted with water (20 mL) and extracted with ethyl acetate (3 x 30 mL); the combined organic layers were washed with saturated aqueous sodium chloride solution (20 mL), dried over sodium sulfate, filtered, and concentratedin vacuo. Preparative thin layer chromatography (Eluent: ethyl acetate) provided the product as a yellow solid. Yield: 120 mg, 253 mmol, 46%. LCMS m/z 475.1 [M+H].

Statistics shows that 3-Bromoimidazo[1,2-b]pyridazine is playing an increasingly important role. we look forward to future research findings about 18087-73-5.

Reference:
Patent; PFIZER INC.; GALATSIS, Paul; HAYWARD, Matthew Merrill; KORMOS, Bethany Lyn; WAGER, Travis T.; ZHANG, Lei; HENDERSON, Jaclyn Louise; KURUMBAIL, Ravi G.; VERHOEST, Patrick Robert; STEPAN, Antonia Friederike; WO2015/92592; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Continuously updated synthesis method about 3814-30-0

The synthetic route of (Bromomethyl)cyclopentane has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 3814-30-0, name is (Bromomethyl)cyclopentane, 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. SDS of cas: 3814-30-0

General procedure: The solution of dihydroxyacetophenone (1, 1.0equiv), anhydrous potassium carbonate (2.0equiv) and corresponding alkyl bromides (2, 1.1equiv) in acetonitrile was stirred at 70-80C for 4-5h. After evaporation of acetonitrile, the reaction mixture was diluted with dichloromethane and washed with water three times. The organic layer was dried with anhydrous sodium sulfate and evaporated under reduced pressure. The crude product was purified by column chromatography to give 3. 6.1.1.9 1-(2-(Cyclopentylmethoxy)-6-hydroxyphenyl)ethanone (3i) Yield 50%; white semi solid; Rf 0.61 (0.5:9.5 EA: HX); IR (KBr) 3239, 2911, 2840, 1614 cm-1; 1H NMR (CDCl3) delta 13.23 (s, 1H), 7.29 (t, J = 8.4 Hz, 1H), 6.52 (dd, J = 0.8, 8.4 Hz, 1H), 6.39 (d, J = 8.2 Hz, 1H), 3.94 (d, J = 7.07 Hz, 2H), 2.70 (s, 3H), 2.33-2.57 (m, 1H), 1.85 (dd, J = 5.73, 6.95 Hz, 2H), 1.52-1.63 (m, 4H), 1.31-1.45 (m, 2H).

The synthetic route of (Bromomethyl)cyclopentane has been constantly updated, and we look forward to future research findings.

Reference:
Article; Venkateswararao, Eeda; Sharma, Vinay K.; Yun, Jieun; Kim, Youngsoo; Jung, Sang-Hun; Bioorganic and Medicinal Chemistry; vol. 22; 13; (2014); p. 3386 – 3392;,
Bromide – Wikipedia,
bromide – Wiktionary

Analyzing the synthesis route of 3972-64-3

According to the analysis of related databases, 3972-64-3, the application of this compound in the production field has become more and more popular.

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. 3972-64-3, name is 1-Bromo-3-(tert-butyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1-Bromo-3-(tert-butyl)benzene

A 1.7 M solution of tert-butyllithium in pentane (2.60 mL, 4.42 mmol) was added to a solution of 1-bromo-3-tert-butyl-benzene (426 mg, 2.00 mmol) in tetrahydrofuran (5 mL) at-78 ¡ãC. After stirring for 1 h, tributyltin chloride (0.57 mL, 2.10 mmol) was added at-78 ¡ãC. After stirring for 18 h, during which time the solution warmed to ambient temperature, the solution was diluted with water and extracted with methylene chloride. The combined organic extracts were dried over magnesium sulfate, filtered, and concentrated to yield 976 mg (115percent yield) of tributyl- (3-tert-butyl-phenyl)-stannane as a impure light yellow oil.

According to the analysis of related databases, 3972-64-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; WO2005/87215; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Sources of common compounds: 337915-79-4

The synthetic route of 337915-79-4 has been constantly updated, and we look forward to future research findings.

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. 337915-79-4, name is 5-Bromo-N1-methylbenzene-1,2-diamine, A new synthetic method of this compound is introduced below., Recommanded Product: 5-Bromo-N1-methylbenzene-1,2-diamine

To a round bottom flask was added 4-bromo-N2-methylbenzene-1,2-diamine (1-2) (9.07 g, 45.1 mmol), sulfamide (8.84 g, 92 mmol), and finally anhydrous pyridine (75 mL). The reaction mixture was then heated to 125C while stirring in a hot oil bath with a water cooled reflux condenser attached under an atmosphere of nitrogen for 14 hours. The crude reaction mixture was then allowed to cool to room temperature, suspended in ethyl acetate and added 6N HCl until pH <3. Crude mixture was then filtered. Filtrate organics were separated, then washed with 6N HCl twice dried over sodium sulfate, filtered, and concentrated to give 6- bromo-1 -methyl- 1,3-dihydro-2,1,3-benzothiadiazole 2,2-dioxide (1-3). HRMS (M+H)+:observed = 262.9486, calculated = 262.9484. The synthetic route of 337915-79-4 has been constantly updated, and we look forward to future research findings. Reference:
Patent; MERCK SHARP & DOHME CORP.; LAYTON, Mark, E.; KELLY, Michael, J.; HARTINGH, Timothy, J.; WO2011/109277; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary