Category: chlorides-buliding-blocks

Related Products of 108-70-3, These common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, 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: An oven-dried and argon-flushed pressure tube was charged with 1,3,5-trichlorobenzene, 1,2,4-trichlorobenzene or 1,2,3-trichlorobenzene (0.25 mmol), Pd2(dba)2 (1.25 mol%), cataCXium A (5.0 mol%), boronic acid (1.5 mmol) and K3PO4 (1.5 mmol) followed by anhydrous toluene (4.0 mL). The tube was sealed with a Teflon valve and the reaction mixture was stirred at 110 C for 24 h. The cooled reaction mixture was diluted with water and extracted with DCM. The combined organic layers were dried (Na2SO4), filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography.

Statistics shows that 1,3,5-Trichlorobenzene is playing an increasingly important role. we look forward to future research findings about 108-70-3.

Reference:
Article; Reimann, Sebastian; Ehlers, Peter; Sharif, Muhammad; Spannenberg, Anke; Langer, Peter; Tetrahedron; vol. 72; 8; (2016); p. 1083 – 1094;,
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Synthetic Route of 2613-34-5, A common heterocyclic compound, 2613-34-5, name is 3-Chloro-2,4-difluoroaniline, molecular formula is C6H4ClF2N, 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.

4-chloro-7-fluoro-6-nitro-quinazoline (5g, 22.0 mmol) obtained in and 3-chloro-2,4-difluoro-aniline (5.39g, 33.0 mmol) were dissolved in 2-propanol (109 mL). The mixture was heated to 80C and further stirred for 4 hours. The mixture was cooled to room temperature, diluted with acetone (100 mL), and stirred for 10 min. The resulting mixture was filtered to the title compound as a solid (7.2 lg, 92%). NMR(300 MHz, CDC13):<5 9.62(s, 1H), 8.47(s, 1H), 7.95(d, 1H), 7.53(s, 1H),7.46(s, 1H)MS(ESI+, m/z): 355 [M+H]+ The synthetic route of 2613-34-5 has been constantly updated, and we look forward to future research findings. Reference:
Patent; HANMI HOLDINGS CO., LTD.; BAE, In Hwan; BYUN, Eun Young; JU, Hae Kyoung; SONG, Ji Young; JUNG, Seung Hyun; JUN, Mi Ae; KIM, Ho Seok; JUNG, Young Hee; SHIM, Mi Yon; AHN, Young Gil; KIM, Maeng Sup; WO2012/30160; (2012); A2;,
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Related Products of 16793-91-2, 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. 16793-91-2, name is 2-Chlorophenethyl Bromide, This compound has unique chemical properties. The synthetic route is as follows.

Compound 28. 1 -(2-chlorophenethyl)-4-(2-methoxyphenethyl)piperidine A 250 mL round bottom flask was equipped with a magnetic stir bar, and then charged with 5 grams (0.0537 mol) of 4-picoline, 8.77 grams (0.0644 mol) of 2- methoxybenzaldehyde, and 50 ml of acetic anhydride. The reaction mass was heated to reflux and maintained at that temperature for 72 hours. The reaction mixture was then cooled to room temperature, and subjected to silica chromatography. Yield of (E)-4-(2- methoxystyryl)pyridine was 7.15 grams (63%). The 7.15 grams of (E)-4-(2- methoxystyryl)pyridine was then charged into a 500 mL hydrogenation flask, to which was added 100 mL of acetic acid as well as 50 mg of Pt02. The reaction mass was subjected to 45 psi of hydrogen gas, and allowed to react at room temperature for 16 hours. The reaction mixture was then filtered through a pad of celite, evaporated, basified with aqueous Na2C03 solution, and extracted with dichloromethane. The combined extraction solvents were removed under reduced pressure via rotovap. The residue was then subjected to silica chromatography, yielding 6.1 grams (82.1 % yield) of 4-(2-methoxyphenethyl)piperidine. A 100 mL round bottom flask equipped with a magnetic stir bar was then charged with 1.0 grams of 4-(2-methoxyphenethyl)piperidine (0.0046 mol), 1 .41 grams of 2- chlorophenethyllbromide (0.0064 mol), 1.87 grams of K2C03 (0.0135 mol), and 20 mL of DMF as solvent. The reaction mass was then heated to 70 C for 24 hours. The excess DMF was removed via reduced pressure, partitioned with water and dichloromethane, the organic layer separated; excess solvent removed under reduced pressure and the residue was subjected to silica chromatography. Yield of l-(2-chlorophenethyl)-4-(2- methoxyphenethyl)piperidine was 1.12 grams (68.0% yield). 1H NMR (300 MHz, CDC13) delta 1.40-1.62 (m, 7H), 2.41-2.75 (m, 10H), 3.84 (s, 3H), 6.92-7.73 (m, 8H) ppm.

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

Reference:
Patent; UNIVERSITY OF KENTUCKY RESEARCH FOUNDATION; CROOKS, Peter, A.; DWOSKIN, Linda, P.; CULVER, John; NICKELL, Justin, R.; ZHENG, Guangrong; WO2014/144064; (2014); A2;,
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Synthetic Route of 2401-24-3, 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. 2401-24-3, name is 2-Chloro-5-methoxyaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

6-(benzyloxy)-3-bromo-2-methylpyridine (ArkPharm catalog No.AK-27978, 0.1 g, 0.360 mmol), 2-(dicyclohexylphosphino)-2′,4′,6′-tri-1-propyl-1,1′-biphenyl (Chemimpex catalog No.27675, 0.013 g, 0.027 mmol), cesium carbonate (0.141 g, 0.431 mmol) and palladium (II) acetate (4.04 mg, 0.018 mmol) were added to a microwave vial containing a stir bar and 5 mL of anhydrous toluene. Then, 2-chloro-5-methoxyaniline (Chemimpex catalog No.27675, 0.059 g, 0.378 mmol) was added. The solvent was degassed with argon twice. The reaction was heated on a heating block to 100 C. for 15 hours. The crude reaction mixture was cooled to room temperature and then filted through celite. The celite was rinsed repeatedly with ethyl acetate to collect the crude product mixture. A normal phase ethylacetate/hexanes column was run on the crude mixture to give 6-(benzyloxy)-N-(2-chloro-5-methoxyphenyl)-2-methylpyridin-3-amine (0.1195 g, 94% yield). 1H NMR (CDCl3, 400 MHz) delta 7.39 (m, 6H), 7.20 (d, 1H, J=8.8 Hz), 6.67 (d, 1H, J=8.4 Hz), 6.26 (dd, 1H, J=2.8, 8.8 Hz), 6.01 (d, 1H, J=2.8 Hz), 5.65 (s, 1H), 5.37 (s, 2H), 3.65 (s, 3H), 2.38 (s, 3H).

The synthetic route of 2-Chloro-5-methoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; OssiFi Inc.; Ellies, Debra; Rey, Jean-Philippe; Kimball, F. Scott; US2014/288068; (2014); A1;,
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These common heterocyclic compound, 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, 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: C6H4ClN3

a) A mixture of 5 g of 5-chlorobenzotriazole, 1.4 g of chloroacetone, 5.1 g of potassium carbonate and 0.5 g of potassium iodide is stirred into 50 mi of acetone at room temperature for 48 h. The mixture is subsequently filtered, the filtrate concentrated by evaporation in a vacuum, and the residue purified by flash chromatography. In this way, two isomeric products, [1- (5-CHLOROBENZOTRIAZOL-1-YI)-PROPAN-2-ONE] and [1-(6-CHLOROBENZOTRIAZOL-1-YL)-] propan-2-one, are isolated in approximately the same quantities, the first of which is then used directly in the next step.

The synthetic route of 5-Chloro-1H-benzo[d][1,2,3]triazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2004/24704; (2004); A1;,
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70558-11-1, name is 6-Chloro-3,4-dihydro-2H-benzo[b][1,4]oxazine, 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. Recommanded Product: 6-Chloro-3,4-dihydro-2H-benzo[b][1,4]oxazine

Reference Example 82 Production of (6-chloro-2,3-dihydrobenzo[1,4]oxazin-4-yl)-(3,5-dibromo-4-hydroxyphenyl)-methanone 6-Chloro-3,4-dihydro-2H-benzo[1,4]oxazine (170.6 mg) obtained in Step 3 of Reference Example 51 and 3,5-dibromo-4-hydroxybenzoyl chloride (349.3 mg) obtained in Step 1 of Reference Example 4 were dissolved in ethyl acetate (5 mL), and the mixture was heated under reflux overnight. The solvent was evaporated, and the obtained solid was crystallized from methanol to give the title compound (441.0 mg) as crystals.

The synthetic route of 70558-11-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Japan Tobacco Inc.; US2008/305169; (2008); A1;,
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Synthetic Route of 112-26-5, 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. 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The synthesis of benzoaza-12-crown-4 is based on the condensation process of o-aminophenol with triethylene glycol dichloride in the presence of sodium hydroxide in the isopropanol medium. 17.4 g of o-aminophenol (0.16 mol) and 12.6 g of sodium hydroxide in 200 ml of isopropanol are placed into a flask, mechanically stirred, and kept at a temperature of 60 C for 60 min. After this 25 ml (0.16 mol) of triethylene glycol dichloride are dropped. The reaction mixture is kept boiling for 20 h. Then the mixture is cooled, acidified with hydrochloric acid to pH 3-4, filtered from inorganic impurities, alkalized with 25% ammonium hydroxide to pH 8-9, and evaporated on a rotary evaporator. The technical product obtained is distilled under vacuum and the high-boiling fraction is separated at a temperature of 150 C and pressure of 6 mm of mercury. The fraction is placed into a sealed vessel and kept at room temperature until the substance transition to the crystalline state. After crystallization the crystals are isolated, washed with acetone, and dried in the air. The product yield is 49 %.

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(2-chloroethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Glushko; Sadovskaya; Blokhina; Anan’Ev; Journal of Structural Chemistry; vol. 56; 1; (2015); p. 142 – 147; Zh. Strukt. Kim.; vol. 56; 1; (2015); p. 149 – 154,6;,
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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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, A new synthetic method of this compound is introduced below., Product Details of 4584-46-7

To a stirred solution of 2-chloro-N,N- dimethylethan-1 -amine hydrochloride (2.00 g, 13.8 mmol) in DMF (20.0 ml_), at r.t under N2atmosphere, was added sodium azide (2.71 g, 41.7 mmol) portion wise over a period of 5 min. After complete addition the reaction mixture was heated at 60 C for 6 h. The reaction mixture was cooled to r. t and the contents were slowly poured onto water (50 ml.) and extracted with MTBE (2 x 100 ml_). The combined organic extracts were washed with brine (100 ml_), dried over anhydrous Na2S04, filtered and concentrated under vacuum to obtain 2-azido-N, N- dimethylethan-1 -amine.

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:
Patent; THE SCRIPPS RESEARCH INSTITUTE; EXPANSION THERAPEUTICS, INC.; DISNEY, Matthew; BLIZZARD, Timothy, Allen; RZUCZEK, Suzanne; NDUNGU, John; VACCA, Joseph; JENNINGS, Andy; PUSHECHNIKOV, Alexei; (333 pag.)WO2019/99777; (2019); A2;,
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Synthetic Route of 2268-05-5, The chemical industry reduces the impact on the environment during synthesis 2268-05-5, name is 2,6-Dichlorofluorobenzene, I believe this compound will play a more active role in future production and life.

4,4,4>,4>,5,5,5′,5′-Octamethyl[2,2′-bi-1,3,2-dioxaborolane] (10.0 g, 39.4 mmol), 2,6- bis(l-methylethyl)-N-(2-pyridinylmethylene)benzenamine (0.40 g, 1.5 mmol), and i-mu- chlorobis[(1,2,5,6- eta)-1,5-cyclooctadiene]diiridium (0.50 g, 1.0 mmol) were added to a solution of 1,3-dichloro-2-fluorobenzene (10.0 g, 60.6 mmol) in heptane (200 mL). The reaction mixture turned from yellow to forest green to brick red within the first minute. The reaction mixture was heated to reflux for 18 h. The mixture was then partitioned between ethyl acetate and water, and the aqueous extract was washed twice with ethyl acetate. The organic extracts were combined, dried over MgSOphi and concentrated under reduced pressure. The solid residue was purified by chromatography on silica gel by elution with ethyl acetate/hexane to afford the title compound as a solid (11.0 g). 1H NMR (CDCl3) delta 7.72 (d, 2H), 1.33 (s, 12H).

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, 2,6-Dichlorofluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; WO2009/51956; (2009); A2;,
Chloride – Wikipedia,
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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. 2106-02-7, name is 2-Chloro-4-fluoroaniline, A new synthetic method of this compound is introduced below., Product Details of 2106-02-7

Acetic anhydride (20 ml) and 2-chloro-4-fluoro-aniline (4.22 g, 29 mmol) were successively added in a 100 ml flask at 100 C for 1 h.After completion of the reaction, the reaction mixture was poured into water, and extracted with ethyl acetate three times, and the organic phase was combined.The organic phase is washed successively with saturated aqueous sodium hydrogencarbonate solution and saturated brine.The organic phase was dried over anhydrous sodium sulfate and concentrated. The title compound was obtained after column chromatography, 2.81 g, yield: 43.29%.

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:
Patent; Jinan University; Ding Ke; Lu Xiaoyun; Mo Cheng; Li Xueqiang; Ren Xiaomei; Zhang Zhang; Tu Zhengchao; Luo Jinfeng; Jie Fuli.bulusi.simeier; Ya Dang.feng.patesen; (30 pag.)CN108503593; (2018); A;,
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