Month: September 2021

Electric Literature of 4152-90-3, A common heterocyclic compound, 4152-90-3, name is (3-Chlorophenyl)methanamine, molecular formula is C7H8ClN, 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.

General procedure: A mixture of amide (5mmol), amine (5mmol), [Ru?NHC] complex (0.5molpercent) and toluene (5mL) was stirred in a sealed tube under nitrogen atmosphere at 110°C for 8h. After cooling down to room temperature, the reaction solvent was removed under vacuum. After removal of the solvent, the crude reaction mixture was dissolved in CH2Cl2 and purified by column chromatography on silica gel (200?400mesh) eluting with heptane:ethanol [25:1] to give corresponding amides as a white solid. The yields are mentioned in Tables 3?5. The product was confirmed by NMR spectroscopy. Reported isolated yields are an average of two runs.

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; Nirmala, Muthukumaran; Prakash, Govindan; Viswanathamurthi, Periasamy; Malecki, Jan Grzegorz; Journal of Molecular Catalysis A: Chemical; vol. 403; (2015); p. 15 – 26;,
Chloride – Wikipedia,
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Application of 106-39-8, 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. 106-39-8, name is 1-Bromo-4-chlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A 50mL round-bottomed flask equipped with a gas inlet tube, a reflux condenser, and a magnetic stirring bar was charged with MCM-41-S-PdCl2 (173mg, 0.05 mmol Pd), aryl halide (5.0 mmol) and HCOONa (7.5 mmol). The flask was flushed with carbon monoxide. DMF (5 mL) was added by syringe and a slow stream of CO was passed into the suspension. The mixture was vigorously stirred at 100-110C for 4-24h, cooled to room temperature, and diluted with diethyl ether (50 mL). The palladium catalyst was separated from the mixture by filtration, washed with distilled water (2×10 mL), ethanol (2×10 mL) and ether (2×10 mL) and reused in the next run. The ethereal solution was washed with water (3×20mL) and dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (hexane-ethyl acetate=10:1). (0008) All formylation products were characterized by comparison of their spectra and physical data with authentic samples. IR spectra were determined on a Perkin-Elmer 683 instrument. 1H NMR (400MHz) and 13C NMR (100MHz) spectra were recorded on a Bruker Avance 400MHz spectrometer with TMS as an internal standard and CDCl3 as solvent.

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-Bromo-4-chlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Hao, Wenyan; Ding, Guodong; Cai, Mingzhong; Catalysis Communications; vol. 51; (2014); p. 53 – 57;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

771583-81-4, name is 4-Chloro-2-(trifluoromethyl)benzylamine, 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. Application In Synthesis of 4-Chloro-2-(trifluoromethyl)benzylamine

4-chloro-2-trifluoromethylbenzylamine (100.0 mg, 0.5 mmol), 1-bromo-2-fluoroethane (78.7 mg, 0.6 mmol) and potassium carbonate (138.2 mg, 1.0 mmol) were dissolved in acetonitrile (5mL),The reaction was heated to 80 C for 4 hours. The reaction solution was cooled to room temperature. The reaction solution was concentrated. The concentrate was purified by preparative thin layer chromatography (eluent: petroleum ether: ethyl acetate = 4: 1 (v: v)) to obtain the title compound (40.0 mg, yield: 30%).

The synthetic route of 771583-81-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Kelun Botai Bio-pharmaceutical Co., Ltd.; Liu Chunchi; Liu Jinming; Cai Jiaqiang; Wang Lichun; Wang Jingyi; (25 pag.)CN110724076; (2020); A;,
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 694-80-4 as follows. category: chlorides-buliding-blocks

General procedure: Step 1: The substituted bromobenzene (1 equiv) and (3-formylphenyl)boronic acid or (4-formylphenyl) boronic acid (1 equiv) were dissolved in a mixture of 1M sodium carbonate aqueous solution (15mL), EtOH (5mL) and toluene (15mL). After nitrogen substitution, Pd(PPh3)4 (0.05 equiv) was added. The reaction mixture was stirred at 80C under nitrogen atmosphere for 12h. The reaction mixture was cooled, and water (15mL) was added. The mixture was diluted with AcOEt (15mL), and the insoluble material was filtered off through Celite. The organic layer of the filtrate was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The residue was purified by silica gel column chromatography using a mixture of petroleum ether/ethyl acetate (10:1, v/v) as eluent to afford the desired product 2a-r, 5a and 5b as a solid. Step 2: To a solution of 2a-r, 5a or 5b (1 equiv) in MeOH (10mL) and THF (20mL) was added portionwise sodium borohydride (3 equiv) at 0C and the mixture was stirred at 0C for 1h. The reaction mixture was pouring into ice water (10mL), and extracted with ethyl acetate (3×15mL), the organic fractions were combined, washed with saturated brine (2×15mL) prior to drying over anhydrous sodium sulfate. After filtration and concentrate using a rotary evaporator, the residue was used in next step without further purification. To a solution of the obtained solid (1 equiv) in dichloromethane (20mL) was slowly added thionyl chloride (6 equiv) and a catalytic amount of DMF at room temperature. After stirring at 40C for 4h, the reaction was concentrated under reduced pressure. The residue was purified by silica gel column chromatography using a mixture of petroleum ether/ethyl acetate (20:1, v/v) as eluent to afford the desired product.

According to the analysis of related databases, 694-80-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Li, Zheng; Liu, Chunxia; Xu, Xue; Qiu, Qianqian; Su, Xin; Dai, Yuxuan; Yang, Jianyong; Li, Huilan; Shi, Wei; Liao, Chen; Pan, Miaobo; Huang, Wenlong; Qian, Hai; European Journal of Medicinal Chemistry; vol. 138; (2017); p. 458 – 479;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1435-50-3, 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. 1435-50-3, name is 2-Bromo-1,4-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Compound 4 – (4 – (1 – (phenyl-sulfonyl) -3 – vinyl – 1H – pyrrolo [2, 3 – b] pyridine -5 – yl) – 1H – pyrazole -1 – yl) piperidine -1 – carboxylic acid tert-butyl ester (205 mg, 0 . 95 mmol), 2 – bromo – 1, 4 – dichlorobenzene (500 mg, 0.9 mmol), Pd (OAc)2 (4 Mg, 0 . 018 mmol), PPh3 (9 Mg, 0 . 036 mmol), K2 CO3 (310 Mg, 2 . 25 mmol), TBAI (0.09 mmol, 33 mg) and anhydrous DMF (5 ml) the mixture under microwave conditions, for 170 C stirring reaction for 1 hour, cooled to the room temperature, the reaction liquid water (15 ml) washing, using EtOAc (10 mLx 3) extraction, the combined organic phase for salt water (30 ml) washing, anhydrous Na2 SO4 Drying, concentrated under reduced pressure, the residue by silica gel column chromatography (PE/EtOAc (v/v)=1/1) to obtain the title compound as a yellow solid (160 mg, 32%).

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-1,4-dichlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; (88 pag.)CN104119331; (2018); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 210532-25-5, 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. 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a 25 mL round bottom flask was added 0.10 g (0.37 mmol, 1.0 eq) of solid JD 1001-002-9, THF 3.2 mL under nitrogen atmosphere.DMAP 0.14 g (1.11 mmol, 3.0 eq), 3,5-difluorobenzenesulfonyl chloride 0.24 g (1.11 mmol, 3.0 eq),The reaction was stirred at room temperature for 3 hours, and the reaction was completed by TLC (developing solvent: PE: EA = 1:1). The reaction was quenched with saturated aqueous NaHCO3 and extracted with ethyl acetate. The organic phase was washed with 0.5N aqueous hydrochloric acid. 2 times, dried anhydrous sodium sulfate, filtered, concentrated organic phase to obtain a solid, separated and purified by high pressure liquid phase (CH3CN:H2O=60:40), lyophilized to obtain about 24mg of product JD1001-2054, the yield is 16% .

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-Difluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Kunming Jida Pharmaceutical Co., Ltd.; Xiao Xuzhi; Zhang Poyong; Lu Faguan; Wang Zhipeng; Chen Mengran; Guo Kun; Zhou Rui; Zhang Yun; (28 pag.)CN109593061; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 174913-12-3, The chemical industry reduces the impact on the environment during synthesis 174913-12-3, name is 1-Bromo-3-chloro-5-methoxybenzene, I believe this compound will play a more active role in future production and life.

Step a: A solution of l-bromo-3-chloro-5-methoxybenzene (835 mg, 3.77 mmol), and l,3,5-trichloro-l,3,5-triazinane-2,4,6-trione (299 mg, 1.29 mmol) in DMF (18 mL) was stirred 16 h under N2 and 50 C. After cooling to RT, the reaction mixture was diluted with aqueous NH4C1 and extracted with Et20. The combined organic phases were dried over MgS04, filtered, concentrated, and the resulting residue was purified by silica chromatography (0 to 25% gradient of EtO Ac/heptane) to l-bromo-2,3-dichloro-5-methoxybenzene (720 mg, 2.81 mmol). 1H NMR (400 MHz, CHLOROFORM-^ delta ppm 7.14 (d, J=2.76 Hz, 1 H), 7.01 (d, J=3.01 Hz, 1 H), 3.81 (s, 3 H).

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-Bromo-3-chloro-5-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NOVARTIS AG; CHEN, Zhuoliang; DORE, Michael; FORTANET, Jorge Garcia; KARKI, Rajesh; KATO, Mitsunori; LAMARCHE, Matthew J.; PEREZ, Lawrence Blas; WILLIAMS, Sarah; SENDZIK, Martin; WO2015/107494; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 367-22-6,Some common heterocyclic compound, 367-22-6, name is 4-Chloro-3-fluoroaniline, molecular formula is C6H5ClFN, 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: A solution of the corresponding 1H-indazole-5-carbaldehyde(2), 1-methyl-1H-indazole-5-carbaldehyde (9) or 1-(2-methoxyethyl)-1H-indazole-5-carbaldehyde (10) (1.0 equiv.),different substituted anilines 3e6 (1.1 equiv.) and acetic acid(0.1 mL/mmol, pH 4e5) in ethanol (3.0 mL/mmol) was stirred underreflux until a precipitation took place. After cooling to roomtemperature, the reaction mixture was sonificated until completeprecipitation. The precipitate formed was filtered and dried at70 C. The crude product was purified by column chromatographyon silica gel (mobile phase: dichloromethane/MeOH 9/1 v/v) andrecrystallized three times from petroleum ether/dichloromethane.

The synthetic route of 367-22-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tzvetkov, Nikolay T.; Stammler, Hans-Georg; Georgieva, Maya G.; Russo, Daniela; Faraone, Immacolata; Balacheva, Aneliya A.; Hristova, Silvia; Atanasov, Atanas G.; Milella, Luigi; Antonov, Liudmil; Gastreich, Marcus; European Journal of Medicinal Chemistry; vol. 179; (2019); p. 404 – 422;,
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. 2106-04-9, name is 3-Chloro-2-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3-Chloro-2-fluoroaniline

4. 0M HCI in Dioxane (4.0 ml) was added to a stirred suspension of 7- (benzyloxy)-4- chloro-6-methoxyquinazoline (CAS Registry NOL62364-72-9, prepared as described in W098/13354, Example 1) (60 g, 0.2 mol) and 3-CHLORO-2-FLUOROANILINE (31.96 g, 0.22 mol) in acetonitrile (1200 ml). The reaction mixture was heated at 80C for 1 hour then left to stand overnight. Acetonitrile (500 ml) was added and the resulting precipitate filtered, washed with acetonitrile (3 x 500 ml) and dried under vacuum to give 7- (BENZYLOXY)-N- (3-CHLORO-2- fluorophenyl) -6-methoxyquinazolin-4-amine hydrochloride as a beige solid (85.45 g, 96%);

According to the analysis of related databases, 2106-04-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2005/26150; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics