Month: March 2021

Reference of 367-21-5, 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 367-21-5 as follows.

(1) 145.6 g (1.00 mol) of 3-chloro-4-fluoroaniline were dissolved in a mixture of 330 ml of 48% strength hydrobromic acid and 330 ml of water and diazotized by adding a solution of 70.4 g (1.02 mol) of sodium nitrite in 220 ml of water dropwise at 5 C. The diazonium salt solution thus obtained was added dropwise to a mixture of 188 g (1.3 mol) of copper(I) bromide and 400 ml of 48% strength hydrobromic acid at 30-40 C. After conclusion of gas evolution, the produce was extracted using three 300 ml portions of hexane. The extracts were washed twice with 5N sodium hydroxide solution and once with water, dried over sodium sulfate and evaporated. The residue yielded 187.2 g (89%) of 4-bromo-2-chlorofluorobenzene of b.p.10 =73-75 C. with a purity >99% (determined by gas chromatography) on subsequent distillation.

According to the analysis of related databases, 367-21-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hoechst Aktiengesellschaft; US4920212; (1990); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 627-42-9, 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. 627-42-9 name is 2-Methoxyethyl chloride, 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.

To a solution of 6 (3.4 g, 20 mmol) in N,N?-dimethylformamide (DMF), K2CO3 (5.5 g, 40 mmol) was added at room temperature. After the mixture was stirred at 90 oC for 10 minutes, the DMF solution (2 mL) of 1-chloro-2-methoxyethane (3.8 g, 40 mmol) was slowly added over the course of 30 min at this temperature. The mixture was stirred at 90 oC for 12 h. After completion of the reaction, the mixture was poured into ice water (60 mL), followed by extraction with ethyl acetate (60 ¡Á 3 mL). The combined organic solvent phase was then washed by water (60 ¡Á 3 mL) and saturated sodium chloride (60 ¡Á 3 mL), dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure to afford an oil, which was purified by column chromatography with petroleum ether/ethyl acetate (10 : 1) to obtain 7. Methyl 2-hydroxy-4-(2-methoxyethoxy)benzoate (7) White solid, yield 91%; mp: 136-138 oC; 1H NMR (CDCl3, 600 MHz): delta = 7.73 (1H, d, J = 8.4 Hz, H-6), 6.48 (1H, dd, J = 1.8, 8.4 Hz, H-5), 6.46 (1H, d, J = 1.8 Hz, H-3), 4.82 (1H, br, ArOH), 4.13 (2H, t, J = 4.8 Hz, ArOCH2), 3.91 (3H, s, COOCH3), 3.75 (2H, t, J = 4.8 Hz, CH3OCH2), 3.45 (3H, s, CH3OCH2); HRMS (ESI) m/z calcd. for C11H14O5 ([M+H]+): 227.0914, found: 227.0913.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Methoxyethyl chloride, and friends who are interested can also refer to it.

Reference:
Article; Liu, Yang; Li, Yijing; Liu, Jianzhen; Yang, Limin; Li, Pengzhan; Zhao, Guisen; Letters in drug design and discovery; vol. 13; 4; (2016); p. 314 – 323;,
Chloride – Wikipedia,
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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 19752-55-7

General procedure: To a flask containing dried LiCl (0.35 g, 8.24 mmol) was added iPrMgCl (2 M in THF, 4.1 mL) and THF (5 mL) at 15¡ã C. After beingstirred for 15 min, 3-bromo-1-benzonitrile (1.46 g, 8.03 mmol) inTHF (1 mL) was added to the reaction mixture and the obtainedmixture was stirred for 15 min. Then, DMF (1.3 mL, 12 mmol) wasadded at 0¡ã C and the mixture was stirred for 2 h. Then, aq NH3 (7 mL, 28-30percent) and I2 (4.06 g, 16 mmol) were added to the reaction mixture. After being stirred for 2 h at room temperature, the reactionmixture was poured into satd aq Na2SO3 solution and was extracted with CHCl3 (3?30 mL). The organic layer was dried over Na2SO4 and filtered. After removal of the solvent, the residue waspurified by short column chromatography on silica gel (eluent:hexane/ethyl acetate=9:1, v/v) to provide pure 1,3-dicyanobenzene (0.73 g) in 71percent yield. Most nitriles mentioned in this work are commercially availableand were identified by comparison with the authentic samples.

According to the analysis of related databases, 19752-55-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ishii, Genki; Harigae, Ryo; Moriyama, Katsuhiko; Togo, Hideo; Tetrahedron; vol. 69; 5; (2013); p. 1462 – 1469;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 10061-02-6, name is trans-1,3-Dichloropropene, 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 10061-02-6, Product Details of 10061-02-6

2-Chloroethylammonium chloride (Entry 1) was reacted with 2-methyl-4-nitrophenyl isothiocyanate according to Method C1a to give the thiazolidine, which was reacted with (E)-1,3-dichloropropene according to Method D2a to give 2-(2-methyl-4-nitrophenylimino)-3-((E)-chloroprop-1-en-3-yl)-1,3-thiazolidine

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, trans-1,3-Dichloropropene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bayer Corporation; US6353006; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 110407-59-5, 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. 110407-59-5, name is 2-Chloro-4-fluorobromobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 1; Synthesis of (+)-4-chloro-2-fluoro-9-trifluoromethyl-9H-fluoren-9-ol (compound No. 526); Step 1; 2′-chloro-4′-fluoro-biphenyl-2-carboxylic acid ethyl ester; To a reaction vessel were added 1-bromo-2-chloro-4-fluorobenzene (25 g), ethyl 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (46 g), toluene (125 ml), water (125 ml) and tripotassium phosphate (50.5 g), and purged with argon. To this mixture was added dichlorobis(triphenylphosphine)palladium(II) (1.67 g) and the mixture was stirred in an oil bath at 110 C. for 3 hr. The oil bath was removed, and water (125 ml) was added to the reaction mixture. The mixture was stirred at room temperature for 1 hr, and filtered through celite. The filtrate was partitioned in a separatory funnel. The aqueous layer was extracted with toluene, and the organic layers were combined. The organic layer was washed twice with water (125 ml), dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to give the title compound (41.8 g). The obtained solid was directly used for the next reaction without further purification.1H-NMR (CDCl3) delta: 8.06-8.02 (1H, m), 7.60-7.54 (1H, m), 7.52-7.45 (1H, m), 7.27-7.16 (3H, m), 7.06-7.00 (1H, m), 4.18-4.09 (2H, m), 1.11-1.06 (3H, m).

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-fluorobromobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; JAPAN TOBACCO INC.; US2010/240634; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 694-80-4, A common heterocyclic compound, 694-80-4, name is 1-Bromo-2-chlorobenzene, molecular formula is C6H4BrCl, 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.

Reference Example 10; 2-(2-Chlorophenyl)-6-methoxy-1,2,3,4-tetrahydroisoquinolin-1-oneTo a solution of 6-methoxy-1,2,3,4-tetrahydroisoquinolin-1-one (1.50 g, 8.5 mmol, obtained in reference example 9) in N-methylpyrrolidone (4 mL) under argon, 1-bromo-2-chlorobenzene (2.34 g, 12.3 mmol), copper (I) iodide (0.33 g, 1.7 mmol) and potassium carbonate (2.33 g, 16.9 mmol) were added and the mixture was heated at 200 C. overnight. It was allowed to cool and CHCl3 and 1N NaOH were added. The phases were separated and the aqueous phase was reextracted 2 times with CHCl3. The combined organic phases were dried over Na2SO4 and the solvent was evaporated. The crude product thus obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford 2.01 g of the desired compound (yield: 77%).LC-MS (method 1): tR=8.05 min; m/z=288.1/290.1 [M+H]+.

The synthetic route of 694-80-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PALAU PHARMA, S.A.; US2010/222363; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 7149-75-9, name is 4-Chloro-3-methylaniline, 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 7149-75-9, SDS of cas: 7149-75-9

Intermediate 6; Step A: Benzyl 4-[(4-chloro-3-methyl-phenyl)carbamoyl]piperidine- 1 -carboxylate.; 1- BenzyloxycarbonyIpiperidine-4-carboxylic acid (1.00 g, 3.80 mmol) and 4-chloro- 3 -methyl – aniline (0.592 g, 4.18 mmol) in C3/4C12 (5 mL) were treated with HOBT (0.582, 3.80 mmol) and EDC (1.46 g, 7.60 mmol), and stirred at rt for 16 h. The mixture was directly purified on Si02 (50 to 100percent EtOAc, hexanes) to afford the title compound. HPLC MS: 387.2/389.1 (M+l); R, = 1.22 min (LC2).

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

Reference:
Patent; MERCK SHARP & DOHME CORP.; GRAHAM, Thomas, H.; LIU, Wensheng; SEBHAT, Iyassu, K.; SHEN, Dong-Ming; SHI, Zhi-Cai; WO2011/156220; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1096296-85-3, A common heterocyclic compound, 1096296-85-3, name is (5-Bromo-2-chlorophenyl)methanamine, molecular formula is C7H7BrClN, 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.

To a solution of (5-bromo-2-chloro-phenyl)methanamine (6.5 g, 29.7 mmol) and triethylamine (TEA) (6 g, 59.4 mmol) in CH2CI2 was added methyl chloroformiate (3.35 g, 35.6 mmol) dropwise at 0 C. Then the reaction mixture was stirred at 25C for 10 hours. The reaction mixture was concentrated, diluted with EtOAc(300 mL), washed with brine, and dried over Na2S04. Concentration under reduced pressure gave methyl N-[(5-bromo-2-chloro- phenyl)methyl]carbamate (4 g, yield 49%).

The synthetic route of 1096296-85-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF SE; WINTER, Christian; RHEINHEIMER, Joachim; WOLF, Antje; TERTERYAN, Violeta; POONOTH, Manojkumar; WIEBE, Christine; KREMZOW-GRAW, Doris; ROeHL, Franz; ROHRER, Sebastian Georgios; WIEJA, Andy; ROSENBAUM, Claudia; GRAMMENOS, Wassilios; WO2014/202703; (2014); 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. 33863-76-2, name is 1-Bromo-3-chloro-5-fluorobenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-3-chloro-5-fluorobenzene

A mixture of 1-bromo-3-chloro-5-fluorobenzene (8Og, 480mmol), zinc cyanide (33.65g, 290mmol) and zinc dust (0.94g, 14.46mmol) in DMF (34OmL) was stirred at rt for 5 min. Dichloro[1 ,1 ‘- EPO bis(diphenylphosphino)ferrocene] palladium(ll) (4.99g, 16mmol) was then added and the mixture was heated under reflux for 50 min. The reaction mixture was cooled to rt and filtered through Arbocel, washing through with diethyl etherpentane (50:50, 7 x 10OmL). The phases were separated and the organic phase was diluted with water (10OmL) and extracted with further diethyl ethe?pentane (50:50, 3 x 10OmL). The combined organic solutions were then washed with water, dried over magnesium sulfate and concentrated in vacuo. Distillation of the residue under reduced pressure afforded the title compound as a colourless solid in 66% yield, 48.5g. LRMS: m/z APCI 155 [MH+]

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; PFIZER LIMITED; WO2006/67587; (2006); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 13918-92-8, 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 13918-92-8 as follows.

To an ice cooled solution of 5′-amino-7′-nitrospiro[cyclobutane-1,3′-indolin]-2′- one (2.0 g, 8.58 mmol) in DCM (20 mL) were added pyridine (1.4 mL, 17.16 mmol) followed by 2,4-difluorobenzenesulfonyl chloride (1.7 mL, 12.87 mmol) dropwise. The mixture was at RT for 3 h. The mixture was diluted with DCM (100 mL), washed with water (100 mL) and brine (100 mL), dried over sodium sulphate and concentrated under reduced pressure to afford the title compound as yellow solid (2.5 g, 89 %.).1H NMR (400 MHz, DMSO-d6): delta 11.0 (s, 1H), 10.86 (s, 1H), 7.95-7.83 (m, 1H), 7.68 (d, J=1.5 Hz, 1H), 7.62 (d, J=1.5 Hz, 1H), 7.56 (t, J=8.8 Hz, 1H), 7.30-7.25 (m, 1H), 2.47-2.40 (m, 2H), 2.35-2.12 (m, 4H).

According to the analysis of related databases, 13918-92-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ORION CORPORATION; UJJINAMATADA, Ravi Kotrabasaiah; SAMAJDAR, Susanta; ABBINENI, Chandrasekhar; MUKHERJEE, Subhendu; LINNANEN, Tero; WOHLFAHRT, Gerd; (220 pag.)WO2016/203112; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics