Category: 108-70-3

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. 108-70-3, name is 1,3,5-Trichlorobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 108-70-3

1,3,5-Trichlorobenzene (3.63 g, 20 mmol) and anhydrous THF (74 mL)were stirred under argon at -78 C and n-BuLi (18 mL, 0.9 M, 16.2mmol) was added dropwise over 30 min. The reaction mixture wasstirred for 1 h. A solution of acetaldehyde (1.76 g, 40 mmol) in anhydrousTHF (2 mL) was added to the mixture dropwise. The reactiontemperature was held at -78 C for 1 h. After 1 h, the reaction wasquenched with H2O and the mixture was transferred to a separatoryfunnel. The organic layer was separated, dried (MgSO4), concentratedby rotary evaporation, and high vacuum to completely remove thevolatiles. The crude product was then submitted to silica gel columnchromatography with hexanes to remove starting material and thenCH2Cl2 to provide the pure alcohol as a colorless oil; yield: 3.66 g(99%).1H NMR (400 MHz, CDCl3): delta = 7.32 (s, 2 H), 5.60-5.50 (dq, J = 6.9, 9.9Hz, 1 H), 2.81 (d, J = 9.9 Hz, 1 H), 1.62 (d, J = 6.9 Hz, 3 H).13C NMR (100 MHz, CDCl3): delta = 137.3, 134.4, 133.5, 129.2, 67.8, 21.3.

The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Miller, Daniel K.; Bailey, Christopher A.; Sammelson, Robert E.; Synthesis; vol. 47; 18; (2015); p. 2791 – 2798;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 108-70-3, name is 1,3,5-Trichlorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,3,5-Trichlorobenzene

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.

The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Reimann, Sebastian; Ehlers, Peter; Sharif, Muhammad; Spannenberg, Anke; Langer, Peter; Tetrahedron; vol. 72; 8; (2016); p. 1083 – 1094;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 108-70-3, A common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, molecular formula is C6H3Cl3, 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.

A 50 mL 3 neck round bottom flask was oven dried, cooled under nitrogen, and char- ged with 14.50 g of xylenes. The flask was then charged with 1,3, 5-TRICHLOROBENZENE (9.760g, 53.49 MMOL), benzophenone imine (7.620 g, 42.04 MMOL), (dba) 3PD2 CATALYST (0.023 g, 0.03 mmol in 2 g xylene), dppf ligand (0.042 g, 0.08 MMOL IN 2 G XYLENE) and sodium t-butoxid (5.550 g, 57.70 mmol). The reaction mixture was heated to reflux (136 C) for 3 hours and then cooled to room temperature. The aromatic imine intermediate was then hydrolyzed with 22 ML OF 2 N HCI (aq) at 70 C for 45 minutes. The hydrochloride salt of dichloroaniline precipitated out of solution when cooled to room temperature. The crude hydrochloride salt was collected by filtration using a buchner funnel and then washed with methyl-tert. butyl ether. The DICHLOROANALINE SALT was then added to 30 mL of METHYL-TERT. BUTYL ether and pH adjusted to 12 using 50% NaOH. The methyl-tert. butyl ether phase was collected and then stripped under va- cuum to give 3, 5-DICHLOROANILINE in 86 % yield.

The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF AKTIENGESELLSCHAFT; WO2004/54961; (2004); A1;,
Chloride – Wikipedia,
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Related Products of 108-70-3, A common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, molecular formula is C6H3Cl3, 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.

A 1 L three-necked flask is charged with 100 g (551 mmoles) of 1,3,5-trichlorobenzene that is placed in suspension in 400 mL of dimethylsulfoxide. This suspension is heated to 80 C., under agitation, then 119.06 g of a 30% solution of sodium methanolate are added drop-wise, i.e. 661.2 mmoles of sodium methanolate. Heating is continued up to 90 C., still under agitation, for 3 hours 10. After this time, the content of the flask is lowered too ambient temperature and it is poured into 4 L of iced water. A white solid is precipitated. This solid is recovered by filtering, washed three times with 250 mL of iced water, then vacuum died at ambient temperature. This gives 95.55 g of 3,5-dichloroanisole in the form of a white powder whose analysis by GC-MS (under the same conditions as previously) shows that it has a degree of purity of 96%. The yield is 98%.

The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Commissariat a l’energie atomique et aux energies alternatives; Pasquinet, Eric; Wuillaume, Anne; Poullain, Didier; Kosciusko-Morizet, Etienne; US2013/178655; (2013); A1;,
Chloride – Wikipedia,
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108-70-3, The chemical industry reduces the impact on the environment during synthesis 108-70-3, name is 1,3,5-Trichlorobenzene, I believe this compound will play a more active role in future production and life.

Example 97.2-(4,6-Dichloro- 1 -methyl- 1 H-indazol-3 -yl)-5H-pyrrolo [2,3 -b]pyrazine-7-carboxylic acid [(R)-2- (3-cyano-azetidin-l -yl)-l -methyl-2-oxo-ethyl]-amide 2,4,6-Trichlorobenzaldehyde was prepared according to the procedure outlined in Synthesis 2008, 279. To a solution of 1 ,3,5 -trichlorobenzene (10.0 g, 55.1 mmol) in THF (200 ml) at -78C was slowly added n-BuLi (1.6 M in hexanes, 34.4 ml, 55.1 mmol) over 20 min. The reaction mixture was stirred at -78C for 30 min then DMF (7.5 ml, 96.4 mmol) was added dropwise. The reaction was stirred at -78C for an additional 1.5 h then quenched with 3 N HC1 (200 ml) and warmed to room temperature. The mixture was extracted with EtOAc. The organic layer was washed with sat NaHCC”3 and brine then dried over MgSC^ and concentrated to afford 10.7 g (93%) of 2,4,6-trichlorobenzaldehyde as a white solid.

The chemical industry reduces the impact on the environment during synthesis 1,3,5-Trichlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; CHEN, Shaoqing; DE VICENTE FIDALGO, Javier; HAMILTON, Matthew Michael; HERMANN, Johannes Cornelius; KENNEDY-SMITH, Joshua; LI, Hongju; LOVEY, Allen John; LUCAS, Matthew C.; LUK, Kin-Chun Thomas; LYNCH, Stephen M.; O’YANG, Counde; PADILLA, Fernando; SCHOENFELD, Ryan Craig; SIDDURI, Achyutharao; SOTH, Michael; WANG, Ce; WOVKULICH, Peter Michael; ZHANG, Xiaohu; WO2013/30138; (2013); A1;,
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A common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, molecular formula is C6H3Cl3, 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. 108-70-3.

General procedure: Palladium(II) acetate (0.025 mmol, 5.6 mg), XPhos (0.0375 mmol, 17.9 mg), and phenylsilatrane (2a, 0.75 mmol, 188.5 mg) were added to a Schlenk flask. The flask was then purged with nitrogen. 4-Chloroanisole (1a) (0.50mmol, 71.3 mg), toluene (1.5 mL), and TBAF (0.75 mmol, 0.75 mL in ca. 1.0 M THF solution) were subsequently added. The mixture was stirred at 100 C for 3 h, then quenched by addition of water, and extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered,and concentrated in vacuo. The crude product was purified by flash column chromatography on silica gel (hexane) to provide 3a (75.2 mg, 0.408 mmol) in 82% yield.

The synthetic route of 1,3,5-Trichlorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yamamoto, Yutaro; Baralle, Alexandre; Godefroy, Anais; Murakami, Kei; Yorimitsu, Hideki; Osuka, Atsuhiro; Heterocycles; vol. 95; 1; (2017); p. 568 – 574;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 108-70-3

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.

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 108-70-3.

Reference:
Article; Reimann, Sebastian; Ehlers, Peter; Sharif, Muhammad; Spannenberg, Anke; Langer, Peter; Tetrahedron; vol. 72; 8; (2016); p. 1083 – 1094;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

108-70-3, name is 1,3,5-Trichlorobenzene, 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. 108-70-3

To a 250 ml single-necked flask was placed 9.5 g (52.4 mmol) of 1,3,5-trichlorobenzene and 100 ml of ultra-dry tetrahydrofuran under argon protection and minus 78 degrees Celsius. Then, 26.3 ml (2 Torr, 52.6 mmol) of lithium diisopropylamide in tetrahydrofuran/n-hexane solution was added dropwise, and the mixture was stirred at minus 78 C for 30 minutes. Then, 10.0 g (47.7 mmol) of Compound A1 was added, and stirring was continued for 2 hours at minus 78 C. The reaction was then slowly warmed to room temperature and quenched by the addition of 200 mL of saturated aqueous ammonium chloride. The combined organic layers were washed with brine (25 mL) After evaporating the solvent, it was purified by column chromatography using methylene chloride: petroleum ether: 1:1 (volume ratio) as eluent to afford 17.5 g of product A2, yield 94%.

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

Reference:
Patent; Jilin University; Li Feng; Ai Xin; Zhang Ming; (25 pag.)CN108191739; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

The chemical industry reduces the impact on the environment during synthesis 108-70-3, name is 1,3,5-Trichlorobenzene, I believe this compound will play a more active role in future production and life. 108-70-3

Example 4; Preparation method of 1,3,5-trifluorobenzene; 500 g of 1,3,5-trichlorobenzene, 1180 ml of sulpholane, 10.7 g of 3-nitrodimethylbenzamide and 640 g of dry KF were initially charged in an autoclave, then 48 g of CNC catalyst were added and the autoclave was sealed. The mixture was heated to 220 C. for 48 h. During the reaction, a maximum total pressure of 8 bar arose. Subsequently, the mixture was cooled to 20 C. The product was distilled off initially at standard pressure, later under reduced pressure. 310 g of a colourless liquid having a proportion of 87% by weight of 1,3,5-trifluorobenzene (74% of theory) and 8.8% by weight of difluorochlorobenzene (6.7% by weight of theory) were obtained. 1,3,5-Trifluorobenzene and difluorochlorobenzene can be separated distillatively in a known manner.

The chemical industry reduces the impact on the environment during synthesis 108-70-3. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Pleschke, Axel; Marhold, Albrecht; US2006/9643; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

108-70-3, 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. 108-70-3, name is 1,3,5-Trichlorobenzene, A new synthetic method of this compound is introduced below.

This is an example of the coupling addition of three aryl groups to a trichloro aromatic hydrocarbon by the catalyst of this disclosure. [0071] The 1 liter coupling reaction flask was equipped as described inexample 3. The flask was charged with anhydrous NiBr2 0.55 grams / 2.5 mmole, TPP 6.55 grams / 25 mmole; 1,3,5-trichlorobenzene 18.31 grams / 0.10 mole and 50 ml / 44.3 grams of reagent grade o-xylene. The green solution of the NiBr2/TPP catalyst was formed by heating the mixture to ref lux and holding at reflux for 30 minutes. After cooling to ambient temperature, 100 ml of dry THE solvent was added. The 500 ml pressure equalizing addition funnel was charged with 320 ml of 1 .0 molar 2-chloromagnesiumtoluenesolution in THE (Aldrich) 0.32 mole. This represents a 3.2/ 1 mole ratio of Grignard / trichloroaryl or about a 7 mole % excess of Grignard. A sample of the starting mixture was taken for gas chromatographic analysis (sample 1). [0072] The coupling reaction was carried out at 50 degrees Celsius by the dropwize addition of the Grignard reactant over 2 hours and 50 minutes.The addition of the Grignard solution turned the mixture to a red-brown color. The mixture was stirred an additional 2 hours at 50 degrees Celsius following the complete addition of the Grignard. Additional samples were taken at 41% of the Grignard addition (sample 2); immediately following the complete addition of Grignard (sample 3); after 2 hours of additional stirring (sample 4)and following the acid hydrogen peroxide quench (sample 5). The table below lists the amount in grams of a given material in the reaction flask on the basis of gas chromatographic analysis. Sample 5 was also submitted for GC-MS analysis for identification of the individual components. This analysis was unable to find any traces of the mono-arylation intermediate product, atestament to the efficiency of the catalyst of this disclosure to poly-arylate multihalogenated aromatic compounds. [0073] The crude product solution was treated with 35 ml of concentrated hydrochloric acid and 115 ml of deionized water, followed by the addition of 3 ml of 50% aqueous hydrogen peroxide. The two liquid phases were separated in a funnel and the yellow organic layer was washed with two 100 ml portionsof 1% aqueous NaCI solution. The organic layer was subjected to nitrogen stripping followed by vacuum at 0.5 kPa pressure while warming the flask to about 50 degrees Celsius to remove all the THE and most of the o-xylene. The sticky solid was dissolved in a mixture of 200 ml of isomeric hexane and 50 ml of toluene. This was passed through a 2.5 cm by 7.5 cm diameter bed ofBrockmann I alumina and the bed washed through with a total of 300 ml of a2/1 v/v mixture of isomeric hexane / toluene. The clear colorless filtrate was stripped with nitrogen to a white sticky waxy solid. This material was recrystallized from 100 ml of refluxing isomeric hexane and cooling to ambient temperature. The white crystals were washed with two 25 ml portions of coldisomeric hexane and dried under 0.5 kPa vacuum. The net weight of pure product was 21.14 grams representing 60% theoretical yield based on 1,3,5- trichlorobenzene.[0074] The proton NMR spectrum ppm relative to TMS: 3H (S) 7.31 ppm 2,4,6 aromatic C-H; 12H (overlapping doublets) 7.30-7.32 ppm aromatic C-Hon outside aromatic rings; 9H (S) 2.415 ppm benzylic CH3.

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; EASTMAN CHEMICAL COMPANY; DEVON, Thomas, James; (41 pag.)WO2018/44824; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics