Month: March 2021

Application of 102-49-8, 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. 102-49-8, name is 3,4-Dichlorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of the 3-cyclohexene-1-carboxaldehyde (375 mg, 3.40 mmol, 1 eq) in 1,2-dichloroethane (8 mL) was treated with the 3,4-dichlorobenzylamine (898 mg, 5.10 mmol, 1.5 eq) and the mixture stirred at rt for 3 hr. Sodium triacetoxyborohydride (1.01 g, 4.77 mmol, 1.4 eq) was then divided into two portions and added to the solution at half-hour intervals, and the solution was left to stir for 18 hr. The reaction mixture was quenched using saturated sodium bicarbonate solution (30 mL) and extracted with ethyl acetate (30 mL). The aqueous layer was further extracted with ethyl acetate (2 x 30 mL) and the combined organic layers were dried over magnesium sulfate, concentrated in vacuo and purified by column chromatography eluting with dichloromethane: methanol (98:2) to yield the product as a pale yellow oil (543 mg, 59percent).

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, 3,4-Dichlorobenzylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Brear, Paul; North, Andrew; Iegre, Jessica; Hadje Georgiou, Kathy; Lubin, Alexandra; Carro, Laura; Green, William; Sore, Hannah F.; Hyvoenen, Marko; Spring, David R.; Bioorganic and Medicinal Chemistry; vol. 26; 11; (2018); p. 3016 – 3020;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 50638-46-5, name is 4-Bromo-3-chloroanisole, 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. Computed Properties of C7H6BrClO

Under argon gas atmosphere, to a solution of 1-bromo-2-chloro-4-methoxybenzene (120 g) in a mixed diglyme (230 mL) and 1,2-dimethoxyethane (90 mL), sodium cyano acetone (62.6 g), sodium t-butoxide (114,6 g) and sodium iodide (81.2 g) were added with stirring at room temperature to obtain a suspension. By another process, under argon gas atmosphere, a mixture of diglyme (40 mL), palladium acetate (426 mg) and triphenylphosphine (1.99 g) was stirred for about 30 minutes at 110C to dissolve. This solution was dropped into the above suspension. The mixture was warmed to 110 to 115C of inside temperature and stirred for 7 hours. The reaction mixture was cooled, diluted with ethyl acetate (480 mL) and washed with an aqueous solution of sulfuric acid (concentrated sulfuric acid 101 g/water 660 mL). The organic layer was washed with 10% saturated aqueous solution of sodium chloride (360 mL) twice. Activated charcoal (3.6 g) was added to the organic layer. The mixture was stirred for 1 hour and filtered. The filtrate was washed with ethyl acetate (240 mL) to obtain a solution of 1-cyano-1-(2-chloro-4-methoxyphenyl)propan-2-on (971.7 g). The yield of the title compound that determined using an internal reference method for HPLC described in Example 1, is 101.7 g.

The synthetic route of 4-Bromo-3-chloroanisole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ONO PHARMACEUTICAL CO., LTD.; EP1637531; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 622-24-2, name is (2-Chloroethyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 622-24-2

To 1-chloro-2-phenylethane (20 g, 0.14 mol) at 0 C was added fuming nitric acid (20 ml) dropwise. The mixture was stirred at the same temperature for an additional 45 min. The reaction was quenched cautiously with water (200 mL). It was extracted with dichloromethane (100 mL), dried over MgSO4, and crystallized from chloroform/hexane to obtain 2 (8.0 g, 30 %).1H NMR (400 MHz, CDCl3) delta 8.20 (d, 2H), 7.40 (d, 2H), 3.75 (t, 2H), 3.20 (t, 2H)

The synthetic route of 622-24-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; WARNER-LAMBERT COMPANY LLC; WO2004/26864; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 75717-77-0, name is 2,4-Dichlorophenylacetylene, 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: C8H4Cl2

General procedure: A mixture of 2-bromonicotinaldehyde (9) (1 equiv, 2.68 mmol), the appropriate alkyne (1.2 equiv, 3.22 mmol), Pd(PPh3)2Cl2 (0.04 equiv, 0.11 mmol), CuI (0.07 equiv, 0.20 mmol), Et3N (1.5 equiv, 4.02 mmol), in dry DMF (16 mL), was stirred under argon atmosphere using microwave irradiation at 60C for 20 min. The reaction mixture was cooled to room temperature, quenched with Et2O (200 mL) and the solid filtered off. The organic solution was evaporated to afford a crude residue which was purified by FC (petroleum ether/AcOEt 8:2).

The synthetic route of 2,4-Dichlorophenylacetylene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Dore, Antonio; Asproni, Battistina; Scampuddu, Alessia; Gessi, Stefania; Murineddu, Gabriele; Cichero, Elena; Fossa, Paola; Merighi, Stefania; Bencivenni, Serena; Pinna, Gerard A.; Bioorganic and Medicinal Chemistry; vol. 24; 21; (2016); p. 5291 – 5301;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 50638-47-6, name is 4-Bromo-2-chloro-1-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 50638-47-6, name: 4-Bromo-2-chloro-1-methoxybenzene

To a THF solution of 4-bromo-2-chloroanisole was added an n-butyllithium/n-hexane solution at -78C, followed by 30 minutes of stirring. Then, trimethyl borate was added and the whole was warmed to room temperature, followed by 30 minutes of stirring. Using the residue obtained by evaporation of the solvent instead of 3,4-dimethoxyphenylboric acid, an objective compound was obtained in a similar manner to Reference Example 1.

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:
Patent; YAMANOUCHI PHARMACEUTICAL CO. LTD.; EP1396487; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 38762-41-3, 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. 38762-41-3, name is 4-Bromo-2-chloroaniline, This compound has unique chemical properties. The synthetic route is as follows.

A. Tert-butyl N-(4-bromo-2-chlorophenyl)carbamate A solution of 4-bromo-2-chloroaniline (5.00 g, 0.0242 mol) in tetrahydrofuran (50 mL) was reacted with a 1.0 M solution of sodium bis(trimethylsilyl)amide in tetrahydrofuran (53.2 mL, 0.0532 mol). The mixture was stirred 15 minutes at ambient temperature. Di-tert-butyl dicarbonate (6.34 g, 0.0290 mol) was added and the solution was stirred for 2 hours. The solvent was removed in vacuo, and the crude material was purified by flash column chromatography on silica using heptane /ethyl acetate (4:1). The solvent was removed in vacuo to give tert-butyl N-(4-bromo-2-chlorophenyl)carbamate as a white solid (4.214 g, 0.0137 mol). 1H NMR (DMSO-d6, 400 MHz) delta 8.75 (s, 1H), 7.71 (d, 1H), 7.54 (d, 1H), 7.50 (dd, 1H), 1.46 (s, 9H);

The chemical industry reduces the impact on the environment during synthesis 4-Bromo-2-chloroaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Abbott Laboratories; US6921763; (2005); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 39989-43-0, A common heterocyclic compound, 39989-43-0, name is 3,5-Dichlorobenzylamine, molecular formula is C7H7Cl2N, 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.

C: N-(3,5-Dichlorobenzyl)-2-nitroaniline A mixture of 2-fluoronitrobenzene (1.2 g, 8.5 mmole) 3,5-dichlorobenzylamine (4.47 g, 25.4 mmole), and ammonium acetate (0.5 g) was reacted substantially as described in 1C above to give 2.5 g (100%) of the title compound as orange crystals: mp 138-140.

The synthetic route of 39989-43-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SmithKline Beckman Corporation; US4728741; (1988); A;,
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. 1303587-99-6, name is 2-Chloro-7,8-dihydro-6H-pyrimido[5,4-b][1,4]oxazine, A new synthetic method of this compound is introduced below., SDS of cas: 1303587-99-6

Synthesis of 2-chloro-8-methyl-7, 8-dihydro-6H-pyrimido [5, 4-b] [I, 4] oxazine [0425] To a stirred solution of 2-chloro-7, 8-dihydro-6H-pyrimido [5, 4-b] [1, 4] oxazine (100 mg, 0.58 mmol) in DMF (5 mL) under argon atmosphere were added potassium carbonate (242 mg, 1.75 mmol) and methyl iodide (0.03 mL, 0.58 mmol) at RT. The reaction mixture was stirred for 16 h. After consumption of the starting materials (monitored by TLC), the reaction was diluted with water (10 mL) and extracted with EtOAc (2 x 10 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was washed with n-hexane (2 x 5 mL) to afford 2-chloro-8-methyl-7, 8- dihydro-6H-pyrimido [5, 4-b] [1, 4] oxazine (28 mg) as a white solid. This compound was used without further purification. 1H-NMR (CD3OD, 500 MHz): delta 7.54 (s, 1H), 4.23-4.20 (m, 2H), 3.60-3.58 (m, 2H), 3.19 (s, 3H); LCMS: 186.1 (M+1); (column; X-Select CSH C-18 (50 x 3.0 mm, 3.5 mupiiota); RT 1.76 min. 0.05% Aq TFA: ACN; 0.80 mL/min); TLC: 50% EtOAc/hexanes (Rf: 0.6).

The synthetic route of 1303587-99-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FORUM PHARMACEUTICALS INC.; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; MCRINER, Andrew, J.; WO2015/66697; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1005-56-7, 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. 1005-56-7, name is O-Phenyl carbonochloridothioate belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of compound 14 (200 mg, 0.47 mmol) in THF (5 mL), was added nBuLi (370 muL, 0.59 mmol, 1 .6 M in hexanes) at -78 C. The resulting solution was stirred at 78 C for 30 min before a solution of O-phenyl chlorothionoformate (100 muL, 125 mg, 0.723 mmol) in THF (1 mL) was added. The resulting mixture was allowed to warm to 0 C and stirred for 3 h before it was quenched with a saturated solution of NH4CI (10 mL) and diluted with CH2CI2 (10 mL). The layers were separated, and the aqueous layer was extracted with CH2CI2 (4 x 5 mL). The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography (silica gel, hexanes: EtOAc 10: 1 ? 5: 1 ) to give compound 15 (243 mg, 92%; mixture of inseparable diastereoisomers) as a yellow oil. (0320) [00240] 1 H NMR (400 MHz, CDCI3) delta = 8.16 (d, J = 7.4 Hz, 1 H), 7.61 – 7.49 (m, 5H), 7.46 – 7.40 (m, 3H), 7.39 – 7.32 (m, 5H), 7.30 – 7.23 (m, 3H), 7.10 (dq J = 1 1 .0, 6.6 Hz, 1 H), 6.82 – 6.77 (m, 2H), 5.28 (s, 2H), 4.68 (d, J = 1 1 .0 Hz, 1 H), 3.12 (s, 3H); 19F NMR (376 MHz, CDCI3) delta = -78.87 (d, J = 6.6 Hz, 3F).

The synthetic route of O-Phenyl carbonochloridothioate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE GOVERNING COUNCIL OF THE UNIVERSITY OF TORONTO; GREIG, Iain; ZANDA, Matteo; TSENG, Chih-Chung; ROSS, Ruth; (134 pag.)WO2016/29310; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 14862-52-3 as follows. Recommanded Product: 14862-52-3

General procedure: A mixture of 1,3-dibromo-5-chlorobenzene (2 g, 7.41 mmol), 9Hcarbazole(2.60 g, 15.56 mmol), tris(dibenzylideneacetone)dipalladium(339 mg, 0.37 mmol), 2-dicyclohexylphosphino-2?,6?-dimethoxy-1,1?-biphenyl (457 mg, 1.11 mmol) and sodium tert-butoxide (2.85 g,29.64 mmol) in 100 ml of toluene were heated at 80 C for 4 h underargon. After cooling down to room temperature, the mixture was extractedwith dichloromethane. The combined organic extracts weredried over Na2SO4 and evaporated under reduced pressure. The crudeproduct was purified by column chromatography on silica gel usingpetroleum ether/dichloromethane (PE/DCM, 8/1, v/v) as the eluent toafford the target compound (2.46 g, 75%).

According to the analysis of related databases, 14862-52-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ran, Quan; Zhang, Yuan-Lan; Hua, Xiaochen; Fung, Man-Keung; Liao, Liang-Sheng; Fan, Jian; Dyes and Pigments; vol. 162; (2019); p. 632 – 639;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics