Month: March 2021

Synthetic Route of 20850-43-5, A common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, molecular formula is C8H7ClO2, 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.

Step 7:Preparation of compound Ig: 2-(Benzo[l,3]dioxol-5-ylmethyl-methyl-amino)-ethanol.2-(Methylamino)ethanol (22.0 g, 290 mmol) was added to a stirred solution of 3,4- methylenedioxybenzyl chloride (25.0 g, 147 mmol) in DCM (45 mL) at -780C under nitrogen. The solution was stirred for 15 minutes at -780C then warmed to room temperature and stirred for 16h. 1.2 M NaOH (100 mL) was added and the phases were separated. The organic layer was washed water (2 x 150 mL) and concentrated under vacuum to give 25.3 g (83%) of 2-(benzo[l,3]dioxol-5-ylmethyl- methyl-amino)-ethanol as a clear oil.

The synthetic route of 20850-43-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KALYPSYS, INC.; WO2007/62417; (2007); A1;,
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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. 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane, A new synthetic method of this compound is introduced below., name: 1,2-Bis(2-chloroethoxy)ethane

Under nitrogen, to the mixture of (22.02 g, 199.98 mmol) in 220 mL of n- butanol, was added 46 mL of aqueous solution of LiOH H2O (18.46 g, 439.94 mmol). The mixture was heated to 95 C, followed by addition of l-chloro-2-[2-(2-chloro-ethoxy)-ethoxy] -ethane (37.43 g, 200.09 mmol) in 240 mL of n-butanol. The reaction was heated overnight, then filtrated. 1 M of aqueous hydrochloric acid was added to adjust pH to 8. After removal of most n-butanol under reduced pressure, the residue was extracted with dichloromethane 250 mL x 2. The combined organic layer was washed with brine and dried over anhydrous MgSCH. The crude product was purified by column chromatography on silica gel, giving 6.5 g of 6,7,9,10,12,13-Hexahydro- 5,8,11,14-tetraoxa-benzocyclododecene as yellow oil, 14.4% yield.

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; ZHIHONG, Chen; (142 pag.)WO2019/46163; (2019); A1;,
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These common heterocyclic compound, 108-41-8, name is 1-Chloro-3-methylbenzene, 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. HPLC of Formula: C7H7Cl

A mixture of 1-chloro-3-methyl benzene (126 mg, 1 mmol), thiophenol (110 mg, 1 mmol), NaOH (60 mg, 1.5 mmol) and 5 mol % NiL2 (38 mg) in DMF was stirred at 70 C for 3 h. The reaction mixture was filtered and the solvent evaporated in vacuo to give the crude product, which was purified by column chromatography (hexane/ethyl acetate=10/1) to give the title compound 3j (152 mg, 76%) as a colourless oil; [Found: C, 77.90; H, 6.12. C13H12S requires C, 77.95; H, 6.04%]; Rf=0.4 (hexane/ethyl acetate=10/1). 1H NMR (400 MHz, CDCl3): delta 7.33-7.21 (m, 9H), 2.33 (s, 3H). 13C NMR (100 MHz, CDCl3): delta 139.6, 136.2, 135.4, 131.7, 130.4, 129.4, 129.1, 128.4, 128.2, 126.7, 21.4.

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

Reference:
Article; Gogoi, Prasanta; Hazarika, Sukanya; Sarma, Manas J.; Sarma, Kuladip; Barman, Pranjit; Tetrahedron; vol. 70; 41; (2014); p. 7484 – 7489;,
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Related Products of 85462-59-5, These common heterocyclic compound, 85462-59-5, name is 2-Bromo-5-chloro-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.

Example 39; 4-Chloro-5-fluoro-2-(4-phenoxy-benzoylamino)-benzoic acid Step 1: N,N-di-tert-Butyloxycarbonyl-2-bromo-5-chloro-4-fluoro-aniline This compound was prepared in analogy to the method of Darnbrough et al. (Synth. Comm. 2001, 31, 3273): Under an atmosphere of Nitrogen, di-tert-butyl dicarbonate [24424-99-5], 8.839 g) was added to a cooled (0 C.) solution of 2-bromo-5-chloro-4-fluoro-aniline ([85462-59-5], 3.03 g) and DMAP (0.165 g) in THF (20 ml). After 4 h at r.t., the reaction mixture was taken up in ethyl acetate, washed with 1N HCl and brine, and dried (Na2SO4). The solvent was evaporated and the residue purified by column chromatography (silica gel, n-heptane, ethyl acetate) to give the title compound (4.66 g, 81%). 1H NMR (CDCl3): delta 1.42 (s, 18H), 7.28 (d, 1H), 7.42 (d, 1H).

The synthetic route of 85462-59-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dehmlow, Henrietta; Grether, Uwe; Kratochwil, Nicole A.; Narquizian, Robert; Panousis, Constantinos; Peters, Jens-Uwe; US2006/281810; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 14862-52-3, 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. 14862-52-3, name is 3,5-Dibromochlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A three neck round bottom flask, equipped with dropping funnel, reflux condenser and magnetic stir bar is charged with an arylhalide (1 eq) and corresponding boronic ester or acid (1.25 eq. per halogen atom in arylhalide), the flask is sealed with a rubber septum, evacuated and backfilled with argon (2 times). Anhydrous dioxane (4ml/mmol of arylhalide) is added through the septum using a double-tipped needle. Separately, a solution of potassium carbonate (2M in water) is prepared and degassed with N2for 30 min. The solution is added to the reaction mixture through the septum using a double-tipped needle, followed by the addition of thetetrakis(triphenylphosphin)palladium(0) (3mol %) under a positive nitrogen pressure. Nitrogen purged reflux condenser is attached to the flask and the reaction mixture is stirred at 90C for 12 h. The mixture is allowed to cool down to the room temperature, a precipitate is collected by filtration, washed with water, methanol, dried in vacuum at 40C to give a crude product, which is further purified by re-crystallization or trituration with appropriate solvents. Final purification is achieved by sublimation in a high vacuum.

The chemical industry reduces the impact on the environment during synthesis 3,5-Dibromochlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; NOVALED GMBH; SENKOVSKYY, Volodymyr; LUSCHTINETZ, Regina; SCHULZE, Benjamin; ROTHE, Carsten; (106 pag.)WO2018/215348; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 623-12-1, name is 1-Chloro-4-methoxybenzene, belongs to chlorides-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 623-12-1, Safety of 1-Chloro-4-methoxybenzene

General procedure: Under an N2atmosphere, KOtBu (1.3 mmol), complex 1 (1 mol%),dioxane (2 ml), amines (1.3 mmol) and aryl chlorides (1.0 mmol)were successively added into a Schlenk tube. The mixture wasstirred vigorously at 90C for 4 h. Then the solvent was removedunder reduced pressure and the residue was purified by columnchromatography on silica gel (eluent:PE/EA = 15:1) to give the pureproducts. The reported yields are the average of two runs.The catalytic reactions have been given in Tables 4-7. The result-ing amines were identified by comparison of the1H and13C NMRdata with those previously reported (ESI).

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:
Article; Nirmala, Muthukumaran; Prakash, Govindan; Ramachandran, Rangasamy; Viswanathamurthi, Periasamy; Malecki, Jan Grzegorz; Linert, Wolfgang; Journal of Molecular Catalysis A: Chemical; vol. 397; (2015); p. 56 – 67;,
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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. 27139-97-5, name is 2-Bromo-4-chloro-1-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H6BrCl

2-Bromo-4-chlorobenzylbromide (5b). To the bromoderivative (6.71 g, 32.68 mmol) (4) dissolved in CCl4 were added N-bromosuccinimide (NBS) (5.82 g, 32.68 mmol), a,a’-azoisobutyronitrile (AIBN) (107.2 mg, 0.65 mmol) and after heating at reflux for 4 hours, the reaction mix- ture was cooled and filtered on Gooch. The filtrate was washed with aqueous sodium thiosulphate solution and then the organic phase was anhydrified on anhydrous sodium sulphate and the solvent evapo- rated. The crude reaction product was purified by flash chromatogra- phy, using n-hexane as the eluent. 6.00 g of product (5b) are thus obtained as a colourless oil with a yield of 64%. ?H NMR (CDCIs) 8 7.58 (d, 1H, J = 1.75 Hz), 7.38 (d, 1H, J = 8.51 Hz), 7.28 (m, 1H), 4.55 (s, 2H); MS m/z 284 (M+), 205 (100), 169,124, 89; Anal. (C7H5Br2CI) C, H, N compliant with the expected structure.

According to the analysis of related databases, 27139-97-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SIGMA-TAU INDUSTRIE FARMACEUTICHE RIUNITE S.P.A.; MINETTI, Patrizia; WO2005/97797; (2005); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 63624-28-2, A common heterocyclic compound, 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, molecular formula is C8H9ClO4S, 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: A mixture of 16a (26.30mg, 0.10mmol), acetyl chloride (7.80mg, 0.10mmol), and pyridine (2.0mL) was stirred at 60C and monitored by TLC. Pyridine was removed under reduced pressure. Then the mixture was basified by 1N NaOH aqueous solution (pH?9), extracted with CH2Cl2 (20mL¡Á3), washed with brine (5mL¡Á3), dried over anhydrous Na2SO4, and concentrated under reduced pressure. The obtained residue was purified by chromatography (petroleum ether/ethanol=8:1, v/v) to afford 2a (0.3g).

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; Song, Pinrao; Chen, Ming; Ma, Xiaodong; Xu, Lei; Liu, Tao; Zhou, Yubo; Hu, Yongzhou; Bioorganic and Medicinal Chemistry; vol. 23; 8; (2015); p. 1858 – 1868;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2613-32-3, name is 2-Chloro-4,5-difluoroaniline, belongs to chlorides-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 2613-32-3, Product Details of 2613-32-3

1-Chloro-4,5-difluoro-2-isothiocyanatobenzene To a mixture of 2-chloro-4,5-difluoroaniline (1 equiv.) and sodium hydroxide (3 equiv.) in DCM (0.24 M) and water (0.24 M) was added dropwise thiophosgene (3 equiv.) at 0 C. The reaction mixture was stirred at 25 C. overnight. TLC showed the reaction was complete. The organic phase was separated and dried over MgSO4, then concentrated to give 1-chloro-4,5-difluoro-2-isothiocyanatobenzene (53%) as a white solid.

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-Chloro-4,5-difluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Signal Pharmaceuticals, LLC; Alexander, Matthew; Bahmanyar, Sogole; Hansen, Joshua; Huang, Dehua; Hubbard, Robert; Jeffy, Brandon; Leisten, Jim; Moghaddam, Mehran; Raheja, Raj K.; Raymon, Heather; Schwarz, Kimberly; Sloss, Marianne; Torres, Eduardo; Tran, Tam Minh; Xu, Shuichan; Zhao, JingJing; Boylan, John Frederick; (317 pag.)US2016/96841; (2016); A1;,
Chloride – Wikipedia,
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These common heterocyclic compound, 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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: 2-Chloro-N,N-dimethylethanamine hydrochloride

NaN3(13.7 g, 210 mmol) was added into a solution of 2-chloro-N,N- dimethylethylamine hydrochloride (10.0 g, 70 mmol) in 100 mL water and the reaction mixture was heated to 70 C for overnight. The solution was basified with 4 M NaOH solution and extracted with anhydrous diethyl ether three times. The resulting solution was dried over MgS04 and concentrated to give volatile colorless oil. (5.9 g, 74%)1H NMR (CDC13, 400 MHz): delta 3.31 (t, 2H), 2.45 (t, 2H), 2.21 (s, 6H, N(CH3)2).

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

Reference:
Patent; CORNELL UNIVERSITY; MA, Minglin; LIU, Qingsheng; (140 pag.)WO2018/140834; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics