Tag: M.W=200-300

Application of 883499-24-9, 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. 883499-24-9, name is 1-Bromo-2-chloro-3-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a nitrogen atmosphere, a flask containing 1-bromo-2-chloro-3-fluorobenzene (10.4 g, 1 eq.), 1OH3NP11D (21.3 g, 50 eq., 1 eq.), potassium carbonate (13.7 g, 2 eq.), and NMP (100 ml) was heated and stirred at 180 C. The reaction liquid was cooled to room temperature, and NMP was distilled off under reduced pressure. Subsequently, water and toluene were added thereto, and the mixture was partitioned. Subsequently, the resulting product was purified by silica gel column chromatography (developing liquid: toluene/heptane=1/1 (volume ratio)), and thus ?1 Br2CL3Px(3NP11D)? was obtained.

The synthetic route of 1-Bromo-2-chloro-3-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kwansei Gakuin Educational Foundation; JNC Corporation; HATAKEYAMA, Takuji; KONDO, Yasuhiro; NAKAMOTO, Keiichi; YANAI, Motoki; (190 pag.)US2018/94000; (2018); A1;,
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Synthetic Route of 14862-52-3, A common heterocyclic compound, 14862-52-3, name is 3,5-Dibromochlorobenzene, molecular formula is C6H3Br2Cl, 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 the round bottom flask was charged with 1,3-dibromo-5-chlorobenzene, 25g (92.47mmol) and 31.3g (184.9mmol) of diphenylamine , into a sodium t- butoxide 26.7g (277.41mmol) was added to 463ml toluene dissolved. Here Pd (dba)2 0.266g (0.462mmol) and tri-tert-butylphosphine was put 0.187g (0.924mmol) in turn and the mixture was stirred under reflux for 4 hours under a nitrogen atmosphere. After the reaction the organic layer was then extracted with ethyl acteate dry distilled over magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The product n- hexane / dichloromethane (9: 1 by volume) to yield the silica gel column 34.7g (84% yield) was purified by chromatography to the desired compound of intermediate M-10 as a white solid.

The synthetic route of 14862-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chei Industries Inc.; Ryu, Dong Wan; Heo, Dal Ho; Jung, Seong Hyeon; Hong, Jin Seok; Kim, Jun Seok; Yoo, Dong Kyu; Lee, Seung Jae; Lee, Han Il; Chang, Yu Na; Cho, Yeong Kyeong; Chae, Mi Yeong; (44 pag.)KR2016/8651; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

13745-86-3, name is 11-Chlorodibenzo[b,f][1,4]thiazepine, belongs to chlorides-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. Application In Synthesis of 11-Chlorodibenzo[b,f][1,4]thiazepine

(b) 11-Piperazinyl-dibenzo[b,f][1,4]thiazepine. Piperazine (1.7 mole) was dissolved in warm toluene (about 50C.) (750 ml) and 11-chloro-dibenzo[b,f][1,4]thiazepine was added. The reaction was heated to reflux and maintained at this temperature for 5 hours. After cooling to ambient temperature the reaction was filtered to remove piperazine hydrochloride, and the organic phase was washed several times with water to remove excess piperazine. The organic phase was dried over magnesium sulfate and after filtration the solvent was removed in vacuo to give the product as an oil. The oil was dissolved in ethanol and treated with a solution of hydrogen chloride in ethanol. 11-Piperazinyl-dibenzo[b,f][1,4]thiazepine was isolated as the dihydrochloride salt in about 88% yield.

The synthetic route of 13745-86-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ICI Americas Inc.; US4879288; (1989); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1-Bromo-4-chloro-2-fluorobenzene

To a stirred solution of 1-bromo-4-chloro-2-fluorobenzene (5 g, 23.87 mmol) in tetrahydrofuran (40 mL) cooled to -78 C was added LDA (14.92 mL, 29.8 mmol) dropwise. The reaction mixture was stirred at this temperature for 30 min. thenallowed to warm to -20 C and stirred for 30 min. The reaction was then cooled to -78 C and trimethyl borate (3.47 mL, 31.0 mmol) dissolved in THF (5 mL) was added dropwise. The reaction mixture was warmed to -20C and stirred for 1 h. The reaction mixture was then cooled to -78 C and peracetic acid (16 mL, 84 mmol) as slowly added dropwise. The mixture was allowed to warm to rt and stirred for 12 h. The reaction mixture was again cooled to 0 C and quenched with 5% ammonium chloride The solution was extracted with ethyl acetate (2×50 mL). The combined organic layers were washed with brine (50 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure to afford 3-bromo-6-chloro-2-fluorophenol (4.99 g, 18.25 mmol, 76 % crude yield) as ayellow oil. The material was carried forward without further purification.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1996-29-8.

Reference:
Patent; Bristol – Myers Squibb Company; Vivekanand, M.Burda; Pan, Senrian; Ramkumar, Rajamani; Sushil, Jetanand Nara; Maheswaran, Shibasanban Calatrava; Tarun Kumar, Meishar; Jonathan, L. Ditta; Carolyn, Diane Jiaba; John, J. Bronson; John, E. Maco; (232 pag.)JP2015/528018; (2015); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

14862-52-3, name is 3,5-Dibromochlorobenzene, belongs to chlorides-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: C6H3Br2Cl

General procedure: 3-bromo-1H-indole (5.0 g, 0.026 mol), 9H-carbazol-3-ylboronic acid (6.5 g, 0.030 mol), Pd(pph3)4 (1.5 g, 0.0013 mol), potassium carbonate (7.2 g, 0.052 mol) in THF 200 ml was reacted at 65 C for 18 hours. After reaction and cooling the H2O:MC after separation of to (n-Hexane: MC) column purification for 1-1 intermediate that is 5.2 g (71% yield) are obtained. (m/z=282). Intermediates 30-2 (4.0 g, 0.010 mol) 1,3-dibromo-5-chlorobenzene to (2.2 g, 0.008 mol) for inserting and removing manufacturing e.g. in the embodiment 1-(1) the same method used in the synthesis of 3.8 g (74% yield) is obtained. (m/z=647)

The synthetic route of 14862-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; P&H tech; Hyeon, Seo Young; Jong, Song Ok; Oh, Hyeon Jin; (92 pag.)KR2015/131700; (2015); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-Bromo-4-chloro-2-fluorobenzene

General procedure: (2-Bromo-5-chloro-phenyl)hydrazine (6) A 250 mLround-bottom flask was charged with 1-bromo-4-chloro-2-fluoro-benzene (8.5 mL,68.0 mmol), hydrazine monohydrate (13 mL, 270 mmol) and dimethylsulfoxide (25mL) and the solution was stirred at 70 C for 3 days. The reaction was then cooled to room temperature and water (200 mL) was added. The precipitate was collected by filtration and dried under vacuum for 16 hours to give (2-bromo-5-chloro-phenyl)hydrazine (14.5g, 65 mmol, 96% yield) as a white solid. LCMS ES+ m/z = 221.0 [M+H]+.

According to the analysis of related databases, 1996-29-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Rene, Olivier; Fauber, Benjamin P.; Tetrahedron Letters; vol. 55; 4; (2014); p. 830 – 833;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 61881-19-4, The chemical industry reduces the impact on the environment during synthesis 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, I believe this compound will play a more active role in future production and life.

General procedure: To an ice cooled suspension of NaH (3.3mmol) in dry THF (20mL) under nitrogen atmosphere was slowly added a solution of the ketone 8a-e(1mmol) in THF (5mL). The resulting suspension was stirred for 30min at 0C and then a solution of the corresponding trifluoroacetimidoyl chloride 9a-e (1mmol) in dry THF (3mL) was slowly added dropwise at 0C and then further stirred at room temperature for 3h. The resulting orange-brown solution was evaporated under reduced pressure, water was added carefully (20mL) and extracted with CHCl3 (2×20mL). The organic extract was separated, dried over anhydrous magnesium sulfate and evaporated obtaining a brown oil, which was further purified either by recrystallization or column chromatography (silicagel, Hex 7: EtOAc 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, 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Romero, Angel H.; Salazar, Jose; Lopez, Simon E.; Journal of Fluorine Chemistry; vol. 169; (2015); p. 32 – 37;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 14862-52-3,Some common heterocyclic compound, 14862-52-3, name is 3,5-Dibromochlorobenzene, molecular formula is C6H3Br2Cl, 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 the round bottom flask was charged with 1,3-dibromo-5-chlorobenzene 25g (92.47mmol) and methyl diphenyl amine 33.9g (184.9mmol) into a sodium t- butoxide 26.7g (277.41mmol) was added to 463ml toluene dissolved. Here Pd (dba)2 0.266g (0.462mmol) and tri-tert-butylphosphine was put 0.187g (0.924mmol) in turn and the mixture was stirred under reflux for 4 hours under a nitrogen atmosphere. After the reaction the organic layer was then extracted with ethyl acetate dry distilled over magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The product n- hexane / dichloromethane (9: 1 by volume) to yield the silica gel column 37.3g (yield 85%) of intermediate M-11 the desired compound is purified by chromatography as a white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,5-Dibromochlorobenzene, its application will become more common.

Reference:
Patent; Chei Industries Inc.; Ryu, Dong Wan; Heo, Dal Ho; Jung, Seong Hyeon; Hong, Jin Seok; Kim, Jun Seok; Yoo, Dong Kyu; Lee, Seung Jae; Lee, Han Il; Chang, Yu Na; Cho, Yeong Kyeong; Chae, Mi Yeong; (44 pag.)KR2016/8651; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 210532-25-5, 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. 210532-25-5 name is 3,5-Difluorobenzene-1-sulfonyl chloride, 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.

1.132 g (5.32 mmol) of 3,5-dif uorobenzene-l-sulfonyle chloride is added under argon to a solution of 545 mg (3.55 mmol) of 5-amino-2-chloronicotinotrile in 20 mL of an anhydrous 1 : 1 mixture of THF and pyridine. The reaction medium is heated to 70C for 3 hours and let 12 additional hours under stirring at room temperature. The solvent is dry evaporated and the crude reaction product is redissolved in ethyl acetate and washed with several aqueous fractions. The organic phase is dried on magnesium sulfate, filtered, concentrated and then purified by silica gel chromatography to yield 784 mg (67%) of N-(6-chloro-5-cyanopyridin-3-yl)-3,5-difluorobenzene-sulfonamide.1H NMR: deltaEta ppm (400 MHz, DMSO) : 1 1,39 (1H, si, NH), 8. 34 (1H, m, CHarom), 8, 10 (1H, m, CHarom), 7,67 (1H, m, CHarom), 7,59 (2H, m, CHarom).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Difluorobenzene-1-sulfonyl chloride, and friends who are interested can also refer to it.

Reference:
Patent; PIERRE FABRE MEDICAMENT; KALOUN, El Bachir; BEDJEGUELAL, Karim; RABOT, Remi; KRUCZYNSKI, Anna; SCHMITT, Philippe; PEREZ, Michel; RAHIER, Nicolas; WO2012/101239; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 60633-25-2, name is 2-Bromo-4-chloro-1-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H6BrClO

Heat a mixture of commercially available 2-bromo-4-chloro-1-methoxybenzene (8.0 g, 36.1 mmol, ), phenol (6.80 g, 72.2 mmol), cesium carbonate (23.54 g, 72.2 mmol), copper (I) chloride (1.79 g, 18.1 mmol) and 2,2,6,6-tetramethyl-3,5-heptanedione (1.66 g, 9.00 mmol) in n-methyl-2-pyrrolidinone (80 mL) at 120 C for 20 h. Cool to room temperature, filter and quench the filtrate with 1 N hydrochloric acid (SO mL). Dilute the filtrate with diethyl ether and extract with water. Dry (sodium sulfate), concentrate and purify (silica gel chromatography, eluting with 90: 10 hexanes: ethyl acetate) to give the title compound 7.42 g (88%).- ¹H NMR (400 MHz, CDCl3) No. 7.35-7.27 (m, 2 H), 7.12-7.05 (m, 2 H), 6.98-6.95 (m, 2 H), 6.93-6.89 (m, 2 H), 3.85 (s, 3 H)

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 60633-25-2.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/100301; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics