Month: July 2021

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. 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C15H14BrClO

Synthesis of compound 63C35H36F206/ C35H34F205I9F NMR (CDCU. 282.5MHz):Hydrate form: -1 17.3 (dd, Jl=257Hz, J2=30Hz, IF, CFF); -125.6 (d, Jl=258Hz, IF, CFF).Ketone form: -112.1 (ddd, Jl=260Hz, J2=32Hz, J3=6Hz, IF, CFF); -119.4 (dd, Jl=260Hz, J2=4Hz, IF, CFF).ass (ESf): 608.4 [M+H20]+; 613.5 [M+Na]+; 619.5 [M+K]+ To a solution of 62 (200mg; 0.35mmol; leq) in dry dichloromethane, under inert atmosphere, was added Dess-Martin periodinane (295mg; 0.70mmol; 2eq). The reaction medium was stirred for 3h at room temperature before a IN aqueous solution of sodium hydroxide (lOmL) was added. The aqueous layer was extracted with dichloromethane and dried over sodium sulphate, filtered and concentrated to afford ketone 63 (158mg, 77% yield) as a light orange solid which rapidly evolves toward the formation of the hydrate form until equilibrium is reached.Synthesis of compound 64C50H49CIF2O6 M=819.37g.mor1 19 F NMR fCDCk 282.5MHz): -1 12.3 (dd, Jl=266Hz, J2=27Hz, IF, CFF); -113.7 (dd, Jl=266Hz, J2=6Hz, IF, CFF).Mass (ESf): 836.7[M+H20]+; 841.8[M+Na]+; 857.7[M+K]+ In a Schlenk tube under inert atmosphere containing magnesium turnings (50mg, 2.04mmol, 1.2eq) was added 2inL (out of 5mL) of a solution of 10 (552mg, 1.70mmol, leq) and 1,2-dibromoethane (15mu, 0.17mmol, O. leq) in dry THF (5mL). The mixture was heated at 75C for 5 min to initiate the reaction and the last 3mL of the solution of 10 and 1,2-dibromoethane were then added dropwise at room temperature. This solution was then stirred at 75C for lh.2.4mL of this Grignard solution, previously cooled to room temperature, were then added to a solution of 63 (158mg, 0.27mmol) in dry THF (2mL). The reaction mixture was stirred at room temperature for 2h before a saturated aqueous solution of ammonium chloride was added. The aqueous layer was extracted with diethyl ether and the combined organic layers were washed with brine, dried over sodium sulphate, filtered and concentrated. The residue was purified on silica gel chromatography (cyclohexane/ethyl acetate 100:0 to 77:23) to afford compound 64 (152mg) as a mixture of two diastereomers with 69% yield. These diastereomers can be separated by semi- preparative HPLC.

The synthetic route of 461432-23-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TFCHEM; DELIENCOURT-GODEFROY, Geraldine; LOPES, Lenaig; WO2012/160218; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 1996-30-1, 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. 1996-30-1 name is 3-Bromo-4-fluorochlorobenzene, 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.

General procedure: 1.00 mmol arylhalide, 1.30 mmol furfural-boronic acid and 0.05 mmolBis(triphenylphosphine)palladium(II) dichloride were treated with 0.30 mLdimethoxyethane, 0.50 mL ethanol and 0.30 mL aqueous 2M sodium carbonate solution.The reaction was heated to 65C for 1h or until the TLC showed no remaining startingmaterial. The mixture was evaporated and extracted three times with ethyl acetate. Thecombined organic layers were washed with brine, dried over MgSO4, filtered andconcentrated. The crude product was purified by column chromatography usinghexanes/ethyl acetate (9:1).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Bromo-4-fluorochlorobenzene, and friends who are interested can also refer to it.

Reference:
Article; Krake, Susann H.; Martinez, Pablo David G.; McLaren, Jenna; Ryan, Eileen; Chen, Gong; White, Karen; Charman, Susan A.; Campbell, Simon; Willis, Paul; Dias, Luiz Carlos; European Journal of Medicinal Chemistry; vol. 126; (2017); p. 929 – 936;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2106-04-9, name is 3-Chloro-2-fluoroaniline, 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 2106-04-9, Safety of 3-Chloro-2-fluoroaniline

Step 1: 6-Acetoxy-4-(3-chloro-2-fluoroanilino)-7-methoxycluinazoline hydrochloride6-Acetoxy-7-methoxyquinazolin-4-one (International Patent Application WO 96/15118, Example 39 thereof; 21.4 kg, 89.3 mol) was suspended in toluene (150 kg). To this was added N-ethyldiisopropylamine (13.3 kg, 103 mol). The brown suspension was heated to 70 C. then phosphorus oxychloride (36.0 kg, 228 mol) was charged. The reaction mixture was stirred at 70 C. for 5 hours. Further toluene (84.0 kg) was added followed by 3-chloro-2-fluoroaniline (14.88 kg, 102 mol). The reaction mixture was stirred at 70 C. for 2 hours during which time a solid precipitated. The suspension was cooled to 25 C. and held at this temperature for 93 hours. The reaction mixture was filtered and the filter cake washed with toluene (2×55.5 kg). The cake was further washed with a mixture of ethanol (24.5 kg) and water (32.0 kg) twice, then ethanol (50.5 kg) twice and the solid then dried under vacuum to give the title product as a beige solid (33.4 kg, 78%); 1H NMR: 2.37 (s, 3H), 4.00 (s, 3H), 7.34 (ddd, 1H), 7.48 (s, 1H), 7.52 (ddd, 1H), 7.61 (ddd, 1H), 8.62 (s, 1H), 8.86 (s, 1H); Mass Spectrum: 362.4, 364.4.

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, 3-Chloro-2-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; US2009/286982; (2009); A1;,
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. 53531-69-4, name is (4-Bromophenyl)methanesulfonyl chloride, A new synthetic method of this compound is introduced below., Application In Synthesis of (4-Bromophenyl)methanesulfonyl chloride

General procedure: Two-step one-pot method: Add bromobenzyl mercaptan to acetonitrile, then add chlorinating reagent, monitor with spot plate, and transfer to ice water bath after reaction.Add 4 equivalents of an acid binding agent such as pyridine.After slowly adding 7-amino-N-propylquinolinone in acetonitrile,The plate is monitored for reaction, after the reaction, pickling, drying,Further, the abscisic acid receptor agonist can be obtained by column chromatography or recrystallization,

The synthetic route of 53531-69-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shaoyang University; Huang Zhiyou; (7 pag.)CN109678797; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 39989-43-0, The chemical industry reduces the impact on the environment during synthesis 39989-43-0, name is 3,5-Dichlorobenzylamine, I believe this compound will play a more active role in future production and life.

Example 124: Synthesis of 4-Chloro-6-(3,5-dichloro-benzylamino)-2H-phthalazin-l- one; A mixture 6-bromo-4-chloro-2H-phthalazin-l-one (97mg, 0.374 mmol), 3,5- dichlorobenzylamine (0.057mL, 0.424 mmol), Pd2(dba)3 (29mg, 0.032 mmol), rac- BINAP (70mg, 0.112 mmol) and NaO’Bu (104mg, 1.08 mmol) in DMA (5mL) was heated at 8O0C for 1.5h. The mixture was allowed to cool, diluted with EtOAc and washed with water. The organic layer was washed with sat.aq. NaHCO3, brine and dried (Na2SO4). Chromatography on silica (EtOAc/hexanes) afforded 4-chloro-6-(3,5-dichloro -benzylamino)-2H-phthalazin-l-one (3 mg) as a white solid, 1H (400 MHz, CDCl3) delta: 4.40 (s, 2H), 6.84 (m, IH), 6.99 (m, IH), 7.22 (m, 3H), 8.14 (m, IH), 10.80 (s, IH) ppm; m/z (M+l) 353.83.

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

Reference:
Patent; FOREST LABORATORIES HOLDINGS LIMITED; WO2008/61108; (2008); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 10272-06-7, name is 3-Chloro-5-methoxyaniline, 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 10272-06-7, Recommanded Product: 10272-06-7

General procedure: To a solution of ethyl 4-bromo-1H-indole-2-carboxylate in toluene underargon atmosphere was added Pd2(dba)3 (0.1 eq), DavePhos (0.2 eq), K3PO4 (3 eq, 1Maqueous solution) and aryl amine (3 eq), and then the mixture was reacted at 80 Cuntil the starting material disappeared. The mixture was cooled to room temperatureand concentrated. Ethyl acetate was added to dissolve the residue and the mixture waswashed with saturated brine and water, dried over anhydrous Na2SO4, andconcentrated in vacuo. The crude product was purified by column chromatography toafford the target compound. Compounds 8a-8f, 8i-8l, 8a-1, 8a-6 ~ 8a-11, 8a-14 wereprepared with method 1.

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

Reference:
Article; Cui, Guonan; Lai, Fangfang; Wang, Xiaoyu; Chen, Xiaoguang; Xu, Bailing; European Journal of Medicinal Chemistry; vol. 188; (2020);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1435-44-5, A common heterocyclic compound, 1435-44-5, name is 1-Chloro-2,4-difluorobenzene, molecular formula is C6H3ClF2, 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.

1-(3-Chloro-2,6-difluoro-phenyl)-carboxaldehyde was prepared from 3-Chloro-2,6-difluorobenzene with lithium diisopropylamide and N,N-dimethylformamide in a method similar to A. S. Cantrell, et al., J. Medicinal Chemistry 1996, 21,4261

The synthetic route of 1435-44-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pfizer Inc; US6342497; (2002); B1;,
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. 102-49-8, name is 3,4-Dichlorobenzylamine, A new synthetic method of this compound is introduced below., Quality Control of 3,4-Dichlorobenzylamine

General procedure: To a solution of the appropriate acid derivative (1 mmol) in dryDMF (5 mL) O-benzotriazol-1-yl-N,N,N’,N’-tetramethyluroniumhexafluorophosphate (HBTU, 2 mmol) was added followed by 1-hydroxybenzotriazole (HOBt, 1 mmol), diisopropylethylamine (DIPEA, 1.5 mmol) and the appropriate amine (1.2 mmol). The mixture was stirred under N2 atmosphere at room temperature for 30 min and DIPEA (1.5 mmol) was added again. The reaction mixture was stirred at room temperature for 18 h, poured into water and extracted with dichloromethane. The organic layer was washed with brine, dried over anhydrous Na2SO4 and evaporated to dryness. The crude product, unless otherwise indicated, was recrystallized from EtOH.#10;

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; Pasquini, Serena; De Rosa, Maria; Ligresti, Alessia; Mugnaini, Claudia; Brizzi, Antonella; Caradonna, Nicola P.; Cascio, Maria Grazia; Bolognini, Daniele; Pertwee, Roger G.; Di Marzo, Vincenzo; Corelli, Federico; European Journal of Medicinal Chemistry; vol. 58; (2012); p. 30 – 43;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 4152-90-3,Some common heterocyclic compound, 4152-90-3, name is (3-Chlorophenyl)methanamine, molecular formula is C7H8ClN, 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: To a mixture of 5a (435mg, 1mmol), HATU (760mg, 2mmol), HOAt (272mg, 2mmol), substituted amine (1.2mmol) and DCM (10mL) at 0°C was added DIPEA (0.52mL, 3mmol), and the reaction mixture was then slowly warm to room temperature and stirred overnight. The reaction was quenched by water and the mixture was extracted with ethyl acetate, washed with water and brine, dried over Na2SO4 and then subjected to flash chromatography

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

Reference:
Article; Gao, Yang; Zhang, Peng; Cui, Anfeng; Ye, De-Yong; Xiang, Meng; Chu, Yong; Bioorganic and Medicinal Chemistry; vol. 26; 20; (2018); p. 5479 – 5493;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 4863-91-6, 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. 4863-91-6, name is 3-Chloro-5-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

j00196j To 4-chlorophenacyl chloride (1.0 g, 5.3 mmol) in anhydrous acetonitrile (15 mL) under a nitrogen atmosphere was added potassium thiocyanate (0.57 g, 5.8 mmol). The suspension was stirred at ambient temperature for 2.5 hours. Next, to the suspension was added 3-chloro-5-fluoroaniline (0.85 g, 5.8 mmol), and the resulting mixture was stirred at ambient temperature for 2 hours. Then, water (30 mL) was slowly added to the reaction mixture, and the resulting mixture was slurried for 20 minutes. The solids were collected by filtration and washed with water then dried in vacuo to yield the title compound (1.72 g, 9 1%).

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

Reference:
Patent; LYCERA CORPORATION; HURD, Alexander, R.; TAYLOR, Clarke, B.; TOOGOOD, Peter, L.; VAN HUIS, Chad, A.; WO2013/185046; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics