Month: August 2021

Electric Literature of 73918-56-6, A common heterocyclic compound, 73918-56-6, name is 2-(4-Bromophenyl)ethanamine, molecular formula is C8H10BrN, 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.

General procedure: The appropriate aldehyde 6a-c and 12a-g (1 mmol) was dissolved in 5 mL of CH2Cl2 in a round bottom flask. Then AcOH (1 mmol) and the appropriate amine (1.1 mmol) were added to the stirring solution at room temperature. The mixture was allowed to stir at room temperature for 20 min before NaBH(AcO)3 (3 mmol) was added. The mixture was allowed to stir at room temperature for overnight. Then,after completion, the reaction was quenched with NaOH 1M solution(15 mL). The mixture was then allowed to stir for 30 min. The reaction mixture was then diluted with EtOAc (10 mL), washed two times with EtOAc (10 mL) and once with brine (20 mL). The organic extracts were collected and then dried over Na2SO4, and the solvent was evaporated to yield the crude compounds 7a-e, 13a-o, 14a-b and 15a which were purified by silica gel column chromatography.

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; Liu, Pingxian; Yang, Yang; Ju, Yuan; Tang, Yunxiang; Sang, Zitai; Chen, Lijuan; Yang, Tao; An, Qi; Zhang, Tianyu; Luo, Youfu; Bioorganic Chemistry; vol. 80; (2018); p. 422 – 432;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 556-96-7, The chemical industry reduces the impact on the environment during synthesis 556-96-7, name is 1-Bromo-3,5-dimethylbenzene, I believe this compound will play a more active role in future production and life.

Copper [(I)] iodide (19 mg, 0.1 mmol), sodium iodide (300 mg, 2.0 mmol) and aryl bromide (1.2 mmol, if solid) were added to a screw-capped test tube with a Teflon-lined septum. The tube was evacuated and backfilled with argon (3 cycles). Dry toluene (1 mL), aryl bromide (1.2 mmol, if liquid) and N, N’-dimethylethylenediamine (0.2 mmol) were added by syringes at room temperature. The reaction was stirred to [110 C] for 24 hours. The reaction mixture was allowed to room temperature and the solvent was removed in [VACUO.] 2-Propanol (1.0 mL, bench top grade without degassing and pre-drying), ethylene glycol (111 [P1L,] bench top grade), aryl thiol (1.0 mmol) and potassium carbonate (276 mg, 2.0 mmol) were added at room temperature. The reaction was heated to 80 [C] and stirred for 18-20 hours. The reaction was allowed to reach room temperature. Ethyl acetate (approx. 5 mL) and dodecane (227 [PL,] GC standard) were added. The organic phase was analyzed by GC and GC-MS. The reaction was then filtered and concentrated. The crude product was purified by column chromatography on silica gel to afford the desired diaryl sulfide product. See Figure 6.

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

Reference:
Patent; MASSACHUSETTS INSTITUTE OF TECHNOLOGY; WO2004/13094; (2004); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 2789-89-1, The chemical industry reduces the impact on the environment during synthesis 2789-89-1, name is 1,2-Bis(4-bromophenyl)ethyne, I believe this compound will play a more active role in future production and life.

Synthesis route a) 1 ,2-bis(4-bromophenyl)-3,4,5,6-tetraphenylbenzene A mixture of tetraphenylcydopentadienone (5.0 mmol), and bis(p-promophenyl) acetylene (5.0 mmol) in diphenyl ether (20 ml) was heated to 260 C overnight. Then the temperature was raised to 270 C. After 69 h, the reaction mixture was cooled, and methanol (100 ml) was added. After stirring for 1 h, the product was filtered off, washed with methanol, and finally dried in vaccuo overnight. Yield: Quantitative.

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, 1,2-Bis(4-bromophenyl)ethyne, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SINVENT AS; PAUCHARD, Vincent Olivier; WO2013/162381; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 52548-00-2, name is 1-Bromo-4-fluoro-2,3-dimethylbenzene, 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 52548-00-2, Recommanded Product: 52548-00-2

B. 3-Fluoro-o-xylene-6-boronic acid To a 125 mL three-necked round-boftomed flask equipped with septum and N2 inlet were added 4.08 g (20 mmol) 3-fluoro-6-bromo-o-xylene and 20 mL dry tetrahydrofuran. The solution cooled to -70 C., and 9.6 mL (24 mmol) of a 2.5 M solution of butyl lithium in hexane was added slowly over 5 minutes. The reaction was stirred 5 minutes at -70 C., then 4.08 mL (24 mmol) triethyl borate added, and stirring continued at -70 C. for 5 minutes. The reaction was then allowed to warm to room temperature and stirred for 16 hours, then poured into dilute hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, and evaporated. The residue was triturated with hexane to a white solid, 2.06 g (64%). 1H-NMR (delta, CDCl3): 2.22 (s, 3H), 2.30 (s, 3H), 6.7-7.3 (m, 2H). 13C-NMR (delta, CDCl3): 25.4, 26.3, 111.5, 111.7, 112.1, 112.3, 124.9, 126.0, 126.1, 130.8, 130.9,159.9,160.6, 162.3,163.0,.

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, 1-Bromo-4-fluoro-2,3-dimethylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; VOLKMANN, ROBERT A.; LOWE III, JOHN A.; NOWAKOWSKI, JOLANTA; US2001/7873; (2001); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 627871-16-3, 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. 627871-16-3, name is 5-Bromo-4-fluoro-2-methylaniline, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of vinylidene chloride (127 ml), tert-butyl nitrite (19 ml) and copper(ll)chloride (18.4 g) in acetonitrile (150 ml) was added a solution of 5-bromo-4-fluoro-2-methyl- phenylamine (Bioorganic &; Medicinal Chemistry Letters (2006), 16(2), 457-460) (21.5 g) in acetonitrile (100 ml) dropwise below 200C. The reaction mixture was stirred at room temperature for 48 hours, poured on diluted HCI and extracted with te/Y-butyl methyl ether (3x). The combined organic layers were washed with brine, dried over sodium sulfate and concentrated. The residue was purified by chromatography on silica gel (ethyl acetate/cyclohexane 1 :4). Yield: 29.20 g of 1-bromo-2-fluoro-4-methyl-5-(2,2,2-trichloro- ethyl)-benzene as an oil. 1H-NMR (CDCI3): delta 2.42 (s, 3H), 3.93 (s, 2H), 7.00 (d, 3J(H,F)=9.2Hz, 1 H), 7.69 (d, 4J(H,F)=7.0Hz, 1 H).

The chemical industry reduces the impact on the environment during synthesis 5-Bromo-4-fluoro-2-methylaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; MUEHLEBACH, Michel; HUETER, Ottmar Franz; WO2010/115780; (2010); 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. 28342-75-8, name is 1,5-Dibromo-2,4-difluorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,5-Dibromo-2,4-difluorobenzene

A cooled (-78 C) solution of diisopropylamine (2.25 mL, 16 mmol) in dry THF (10 mL) was treated with n-BuLi (10 mL, 16 mmol, 1.6 M) and then allowed to warm to room temperature. This LDA solution was added drop wise to a solution of l,5-dibromo-2,4- difluorobenzene (3.50 g, 13 mmol) in dry THF (20 mL) at -78 °C. The solution was stirred at -78 °C for 20 minutes, dry C02(g) was bubbled through it, it was warmed to room temperature and dil HCl (10 mL) was added, extracted to DCM, dried (MgS04) and evaporated. Yield (2.73 g, 67 percent) as a pale white solid. 1H NMR (CDC13): delta 8.35 (1H, t, J=9 Hz).

The synthetic route of 28342-75-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CAMBRIDGE DISPLAY TECHNOLOGY LIMITED; SUMITOMO CHEMICAL COMPANY LIMITED; STEUDEL, Annette; KOZHEVNIKOV, Valery; WO2014/9715; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 22034-13-5, name is 4-Bromobenzo[c][1,2,5]thiadiazole, 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 22034-13-5, Computed Properties of C6H3BrN2S

In a first step, 10 g (73.52 mmol) of 2,1,3-benzothiadiazole (1) was added to a 100 ml round-Suspended in 50 ml HBr solution (48percent),A solution of 2.8 ml (54.26 mmol) of bromine was added dropwise with vigorous stirring,After all the drops were added, the mixture was heated to 150 ° C and refluxed for 2 hours.After completion of the reaction, the mixture was cooled to room temperature,The reaction mixture was poured into 500 ml of water,The precipitated solid was filtered to give 10.4 g of crude product;The crude product contains a small amount of dibromo substituted product as well as the starting material.The crude product is directly put into the next step.Under nitrogen protection,To a 500 ml two-necked round bottom flask equipped with a condenser tube was added 8.556 g of crude product (assuming all 4-bromo-2,1,3-benzothiadiazole (2), 40 mmol)10.208 g (44 mmol) of 4-formylphenylboronic acid pinacol ester,2.32 g (2.0 mmol) of tetrakis (triphenylphosphine) palladium and 200 ml of THF,Followed by the addition of 200 ml of an aqueous solution of potassium carbonate (11.06 g, 80 mmol), heated to reflux and stirred for 12 h.After completion of the reaction, the mixture was cooled to room temperature and the mixture was extracted three times with dichloromethane. The separated organic layer was dried over anhydrous sodium sulfate. The crude product obtained by distilling off the solvent under reduced pressure was treated with dichloromethane / petroleum ether (2: 1) as the eluent,Silica gel column chromatography afforded 8.2 g of pale yellow 4-formylphenyl-2,1,3-benzothiadiazole (3).

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-Bromobenzo[c][1,2,5]thiadiazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jiangnan University; Ye, Jun; Liu, Huan; Zhang, Mingfei; (15 pag.)CN106588935; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 766-46-1, These common heterocyclic compound, 766-46-1, name is 2′-Bromophenylacetylene, 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.

In an appropriate amount of organic solvent DMSO,Adding 100 mmol of the compound of the above formula (I),170 mmol of the compound of the above formula (II),5 mmol two-component composite catalyst (a mixture of 1.5 mmol PdCl 2 (cod) and 3.5 mmol ferrocene), 18 mmol of the above ligand L1130 mmol of oxidant m-chloroperoxybenzoic acid and 25 mmol of acid promoter trifluoroacetic acid,After joining,The temperature was raised to 45 C and the reaction was stirred at this temperature for 6 hours.After the reaction is over,Cool naturally to room temperature,filter,The filtrate was washed thoroughly with deionized water and then with acetic acidEster extraction 2-3 times,Combine the organic phase,And dried over anhydrous magnesium sulfate,Concentrated under reduced pressure,The residue was separated by silica gel column chromatography.An equal volume ratio of a mixture of n-pentane and acetone is used as an elution solvent.Thereby obtaining a compound of the above formula (III),The yield was 96.7%.

The synthetic route of 766-46-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Yancheng Geruiyin Chemical Co., Ltd.; Ding Gang; (10 pag.)CN105130769; (2018); B;,
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. 766-81-4, name is 3-Bromophenylacetylene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 766-81-4

General procedure: Step1: A mixture of Zn (3 mmol, 196.1 mg, activated by washing with dilute HCl) MeI(6 mmol, 851.6 mg) or EtI (6 mmol, 935.8 mg), phenylacetylene (2 mmol, 204.3mg) and NMP(0.5 mL) was stirred at room temperature until Zn disappeared (~ 2 h). Step 2 CH2Cl2(5 mL) and alpha-ketoneester (0.5 mmol) (oran aldehyde ) wereadded to the mixture of step 1 and the reaction was allowed to proceed at room temperature. After stirredfor ~12 h, the reaction was shown to be complete by TLC. A saturated ammonia chloride solution (10 mL)was added and the organic phase was separated.The water phase was extracted with CH2Cl2. The combined organic phase was washed withsaturated sodium chloride solution and dried with anhydrous sodiumsulfate. After concentration and column chromatograph on silica gel eluted with petroleumether/ethyl acetate (10:1), the product was obtained.

According to the analysis of related databases, 766-81-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Wen; Cao, Yuan; Chen, Wei; Zhao, Gang; Pu, Lin; Tetrahedron Letters; vol. 56; 46; (2015); p. 6430 – 6432;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 10546-67-5, These common heterocyclic compound, 10546-67-5, name is 2,6-Dibromo-4-(tert-butyl)aniline, 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.

Take 3g of 2,6-dibromo-4-tert-butylaniline, 80mg of PdCl2(PPh3)2, 40mg of CuI, add 100mL of triethylamine, under argon protection, then slowly add 840mg of 2-methyl-3- Butyn-2-ol was stirred at 50 C for 60 hours. After the solution was cooled to room temperature, ethyl acetate was added to the reaction mixture, which was filtered. Then, it was extracted with dichloromethane and water, and the solvent was evaporated from dichloromethane.4-(2-Amino-3-bromo-5-(tert-butyl)phenyl)-2-methylbut-3-yn-2-ol(Compound of the formula (III)).

The synthetic route of 10546-67-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanxi Datong University; Yuan Yuehua; Zhu Yongjun; Tian Maozhong; Chen Zezhong; Qin Jun; Feng Feng; (15 pag.)CN109810019; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary