Category: chlorides-buliding-blocks

38762-41-3, name is 4-Bromo-2-chloroaniline, 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. HPLC of Formula: C6H5BrClN

[00402] Synthesis of (4′-amino-3′-chlorobipheyl-4-yl)(4, 4-difluoropiperidin-l- yl)methanone (58): A mixture of 4-bromo-2-chlorobenzenamine (57; 2 g, 9.7 mmol), (4,4- difluoropiperidin-l-yl)(4-(4,4,5,5-tetramethyl-l,3,2-dioxaborolan-2-yl)phenyl)methanone (4.1 g, 11.6 mmol), Pd(dppf)Cl2 (709 mg, 0.97 mmol), and K2C03 (2.7 g, 19.4 mmol) in 100 mL of dioxane and 10 mL of H20 was stirred at 100 C under nitrogen atmosphere for 2 h. The reaction mixture was cooled to room temperature and extracted with EtO Ac (100 mL X 3). The combined organic layers were washed with brine, dried over anhydrous Na2S04 and filtered, and the filtrate was concentrated under reduced pressure to give crude product, which was purified by silica gel chromatography (25% EtO Ac/petroleum ether) to yield 3.1 g of (4′-amino-3′-chlorobipheyl-4-yl)(4, 4-difluoropiperidin-l-yl)methanone (58) as a yellow solid (yield 91%). LCMS: m/z 351.1 [M+H]+, tR = 1.84 min.

The synthetic route of 38762-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KARYOPHARM THERAPEUTICS INC.; BALOGLU, Erkan; SHACHAM, Sharon; SENAPEDIS, William; (155 pag.)WO2017/31204; (2017); A1;,
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Adding a certain compound to certain chemical reactions, such as: 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane, 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 112-26-5, HPLC of Formula: C6H12Cl2O2

A mixture of imidazole (32 mmol, 2.176 g) and potassium hydroxide (32 mmol, 1.792 g) in DMSO (25 ml) was stirred at 70 C for 1 h. After this time, 1,2-bis(2-chloroethoxy)ethane (16 mmol, 2.48 ml) was added to the reaction mixture and stirred for 24 h. The resulting mixture was poured into 100 mL of water and extracted with methylene chloride (5 x 20 ml). The combined organic layer was washed with water (3 x 20 ml), dried with anhydrous Na2SO4, and concentrated to give 1,2-bis(2-(1H-imidazol-1-yl)ethoxy)ethane (1) as a pale yellow viscous oil, 3.10 g, 77 % yield

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; Eshghi, Hossein; Rahimizadeh, Mohammad; Hasanpour, Maede; Bakavoli, Mehdi; Research on Chemical Intermediates; vol. 41; 7; (2015); p. 4187 – 4197;,
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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. 59681-66-2, name is 4-Chloro-N1-methylbenzene-1,2-diamine, A new synthetic method of this compound is introduced below., Safety of 4-Chloro-N1-methylbenzene-1,2-diamine

General procedure: General procedure for the synthesis of 2-mercaptobenzimidazole derivatives (18-34): the proper 1,2-phenylenediamine 1-17 (16 mmol) was added over a stirred solution of ethanol (50 mL), water (5 mL), potassium hydroxide (19.2 mmol) and carbon disulfide (19.2 mmol). The mixture was heated overnight under a N2 atmosphere at 50 C. The cold reaction mixture was then neutralized with acetic acid and poured into 250 mL of cold water for complete precipitation. The solid was separated and dried using vacuum filtration. The crude product was purified by recrystallization, adding norite to the solvent.

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; Perez-Villanueva, Jaime; Hernandez-Campos, Alicia; Yepez-Mulia, Lilian; Mendez-Cuesta, Carlos; Mendez-Lucio, Oscar; Hernandez-Luis, Francisco; Castillo, Rafael; Bioorganic and Medicinal Chemistry Letters; vol. 23; 14; (2013); p. 4221 – 4224;,
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Electric Literature of 98-60-2, 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. 98-60-2, name is 4-Chlorobenzenesulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: 4-Methoxybenzenesulfinic acid sodium salt (1j) was prepared by heating 2.5 g of sodium sulfite, 2.06 g of 4-methoxybenzenesulphonyl chloride, and 1.68 g of sodium bicarbonate in 9.6 mL of water at 70-80 C for 4 h. After cooling to room temperature, water was removed under vacuum and the residue was extracted by ethanol, recrystallization as a white solid, the yield was 67% (1.34 g). Similarly, other sodium arenesulfinates were prepared from their corresponding sulphonyl chlorides.

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, 4-Chlorobenzenesulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Tian, Heng; Cao, Aijuan; Qiao, Lijun; Yu, Ajuan; Chang, Junbiao; Wu, Yangjie; Tetrahedron; vol. 70; 47; (2014); p. 9107 – 9112;,
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Synthetic Route of 118-69-4, A common heterocyclic compound, 118-69-4, name is 2,6-Dichlorotoluene, molecular formula is C7H6Cl2, 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.

Ammoxidation runs were carried out in a fixed bed tubular quartz reactor, which is filled with 5g of catalyst particles prepared by the methods described in examples 1 to 3 and mixed with corundum particles of the same size in 1: 1 by weight ratio. A preheating zone is provided on the top of the catalyst bed. The catalyst was activated in a mixture of air and [NH3] at [400C] for 4 hours and then the catalytic runs were performed. The 2,6-DCT and [H20] were pumped in the mole ratio of 1: 15 to 20. The product stream was collected for every half-an-hour and analysed by gas chromatography. The reaction was carried out under the following reaction conditions. A reaction temperature of 350 to [400C] was used, and the GHSV comprised between 650-750 [H-‘.] The contact time consisted of 4.8 to 5.5 seconds. The mole ratio of 2,6-DCT : H20 : NH3: air was 1: 15: 3-4: 21, the molar concentration of 2,6-DCT was 2.4 % and the ratio of O/NH3 was 1. [1 %.]

The synthetic route of 118-69-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TESSENDERLO CHEMIE S.A.; WO2003/101939; (2003); A2;,
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Application of 697-86-9, These common heterocyclic compound, 697-86-9, name is 2-Bromo-4,6-dichloroaniline, 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.

g) [(2,4-dichloro-6-bromophenyl)-hydrazono]propanedinitrile, mp 134-136 C. from 2,4-dichloro-6-bromoaniline (Eur. J. Med. Chem. Clin. Therap. 12, 361 [1977])

Statistics shows that 2-Bromo-4,6-dichloroaniline is playing an increasingly important role. we look forward to future research findings about 697-86-9.

Reference:
Patent; Boehringer Mannheim GmbH; US5215924; (1993); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, 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 4090-55-5, Recommanded Product: 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide

In a reflux condenser, thermometer, stirrer,Constant pressure dropping funnel 2000mL four-necked flask was added74g cyclic phosphorus oxychloride,8g anhydrous aluminum trichloride and800mL chloroform,Under stirring to make it fully dissolved.Under stirring at 10 C,22.8g of cyclohexanediamine was added to a four-necked flask,To be added after completion of cyclohexanediamine, the temperature was raised to 50 , and at this temperature for 8h,After the reaction was completed, the solvent was recovered by distillation under reduced pressure, the residue was washed with deionized water three times,A white solid powder was obtained, which was dried at 60 C for 10 h to give 72.5 g of the product in a yield of 88.8% by weight.

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; Sinopec Corporation; Sinopec Corporation Fushun Petrochemical Institute; Zhao Wei; Wang Xiaolin; Li Ming; Liu Mingrui; Xue Qian; (8 pag.)CN104558039; (2017); B;,
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Application of 626-43-7,Some common heterocyclic compound, 626-43-7, name is 3,5-Dichloroaniline, molecular formula is C6H5Cl2N, 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.

To a solution of benzoyl isothiocyanate (1.01 g, 6.17 mmol, Eq: 1.00) in acetone (15 mL), was added 3,5-dichloroaniline (1 g, 6.17 mmol, Eq: 1.00). The reaction mixture was heated at 40C for 3 hr. TLC shows starting material. The reaction was heated to 50C overnight. The reaction was cooled to room temperature, and carefully poured into ice water (pH 5). The resulting sold was filtered, washed with water, and dried to give 1.85 g (92%) of desired product as an off- white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,5-Dichloroaniline, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; DING, Qingjie; JIANG, Nan; WEIKERT, Robert James; WO2014/135472; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, molecular formula is C5H10ClO3P, 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-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide

(2R,3R,4R, 5R)-5 -((((((2R,3R,4R, 5R)-5-(6-Benzamido-9H-purin-9-yl)-4-((tert- butyldimethylsilyl)oxy)-2-(hydroxymethyl)tetrahydrofuran-3 -yl)oxy)(2-cyanoethoxy)phosphoryl)oxy)methyl)-4-((tert-butyldimethylsilyl)oxy)-2-(4-oxo-4, 5 -dihydro1 H-imidazo [4,5 -c]pyridin- 1 -yl)tetrahydrofuran-3 -yl hydrogen phosphonate (160 mg) was subjected to azeotropic dehydration with anhydrous pyridine, and anhydrous pyridine (3.0 mL) was added thereto. To the mixture was added 2-chloro-5,5-dimethyl-1,3,2- dioxaphosphinane 2-oxide (99 mg) at room temperature, and the mixture was stirred at room temperature for 1 hr. Water (96 1iL) and iodine (50.5 mg) were added thereto, and the mixture was stirred at room temperature for additional 20 mm. To the reaction mixture was added a mixture of sodium thiosulfate (190 mg) and water (0.4 mL), and the mixture was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methanol/ethyl acetate) to give the title compound (10.6 mg). MS: [M+H] 1044.3

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4090-55-5, its application will become more common.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; YOSHIKAWA, Masato; SAITOH, Morihisa; KATO, Taisuke; YOSHITOMI, Yayoi; SEKI, Tomohiro; NAKAGAWA, Yasuo; TOMINARI, Yusuke; SETO, Masaki; SASAKI, Yusuke; OKANIWA, Masanori; ODA, Tsuneo; SHIBUYA, Akito; HIDAKA, Kosuke; SHIOKAWA, Zenyu; MURATA, Shumpei; OKABE, Atsutoshi; NAKADA, Yoshihisa; MOCHIZUKI, Michiyo; FREEZE, Brian Scott; TAWARAISHI, Taisuke; WADA, Yasufumi; GREENSPAN, Paul D.; (423 pag.)WO2018/100558; (2018); A2;,
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Reference of 61881-19-4,Some common heterocyclic compound, 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, molecular formula is C8H5ClF3N, 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.

Perbenzoylated glucopyranoside (2.00 g, 2.85 mmol) was dissolved in CH2Cl2 (10 mL) followedby addition of 30% HBr/AcOH (1.33 mL). The reaction mixture was stirred for 3 h and thenpoured into ice water (100 mL). The aqueous phase was extracted with CH2Cl2 (2×50 mL). Thecombined organic phases were dried over MgSO4, filtered and concentrated. Without furtherpurification the off-white solid was dissolved in acetone (10 mL) and H2O (0.5 mL). Ag2CO3 (0.404 g, 1.46 mmol) wasadded and the reaction mixture was stirred for 2 h at 22 C. The suspension was filtered through a plug of celite andconcentrated to give the product in quantitative yield. Rf 0.36 (2:1 heptane/EtOAc).The residue was dissolved in CH2Cl2 (20 mL). The solution was cooled to 0 C followed by addition of PTFAICl (1.18 g,5.70 mmol) and Cs2CO3 (1.86 g, 5.70 mmol). The reaction was stirred at 0 C for 5 h. The reaction was filtered,concentrated and the crude was purified by flash chromatography (9:1 Tol/EtOAc) to give the product 9 as a whitepowder. Yield: 1.73 g (79% over two steps)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, its application will become more common.

Reference:
Article; Andersen, Mathias C.F.; Boos, Irene; Marcus, Susan E.; Kra?un, Stjepan K.; Rydahl, Maja Gro; Willats, William G.T.; Knox, J. Paul; Clausen, Mads H.; Carbohydrate Research; vol. 436; (2016); p. 36 – 40;,
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