Month: July 2021

Synthetic Route of 13918-92-8,Some common heterocyclic compound, 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, molecular formula is C6H3ClF2O2S, 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.

Intermediate 4Preparation of lambda/-(5-bromo-3-pyridinyl)-2,4-difluorobenzenesulfonamide To a cold (0 0C) stirred solution of 3-amino-5-bromopyridine (18.6 g, 107.4 mMol) in dry pyridine (100 mL) was added 2,4-difluorobenzenesulfonyl chloride (25 g, 112.8 mMol) over 3 minutes. The reaction mixture was stirred at 0 0C for 1 h and evaporated to dryness under vacuum. The residue was diluted with H2O (400 mL) and EtOAc (400 mL). The organic layer was washed with H2O and brine, and the combined aqueous layers were extracted with EtOAc (100 mL). The combined extracts were dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was dissolved in boiling EtOAc (200 mL), and placed in a freezer for 2 days. Two crops were obtained through filtration, which were combined and triturated with boiling 35% EtOAc in hexanes. After cooling to room temperature, the precipitate was collected by filtration and dried to constant weight to provide 27.2 g of iV-(5-bromo-3-pyridinyl)-2,4- difluorobenzenesulfonamide as a light orange solid. MS (ES) m/e 351.0 (M + H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4-Difluorobenzene-1-sulfonyl chloride, its application will become more common.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2008/157191; (2008); A2;,
Chloride – Wikipedia,
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Related Products of 13918-92-8, The chemical industry reduces the impact on the environment during synthesis 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, I believe this compound will play a more active role in future production and life.

General procedure: To the solution of meridianin G (7) or meridianin C (3) indichloromethane (5 ml) was added DMAP (0.05 equiv.), aryl/heteroarylsulfonyl chloride (1.1 equiv.) and N,N-diisopropylethylamine(1.5 equiv.). The mixturewas stirred at room temperature for20 h. Reaction was then quenched by the addition of 10% HCl. Thisreaction mixture was extracted with dichloromethane (50 ml 3),and combined organic layer was evaporated on rotary evaporator.Purification by silica gel column chromatography (mesh 100e200)using dichloromethane-methanol (99:1 to 97:3) to get the titledproducts 14aead.

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, 2,4-Difluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Yadav, Rammohan R.; Khan, Shabana I.; Singh, Samsher; Khan, Inshad A.; Vishwakarma, Ram A.; Bharate, Sandip B.; European Journal of Medicinal Chemistry; vol. 98; (2015); p. 160 – 169;,
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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 2770-11-8 as follows. Recommanded Product: 2770-11-8

General Procedure for the Microwave-Assisted Preparation of the Final Piperidine Compounds.To a solution of 2-(4-chlorophenoxy)benzenamine (100 mg, 0.46 mmol), the relevant N-Acetyl-2-substituted-4-piperidone (0.92 mmol) and sodium triacetoxyborohydride (241 mg, 1.14 mmol) in DCE (1.5 ml) in a MW tube, was added acetic acid (83 mg, 1.38 mmol). The MW tube was sealed and heated at 14O0C for 10 rnins in a CEM discoverMW instrument. The reaction was quenched with a saturated aqueous solution of sodium bicarbonate (10 ml) and extracted with ethyl acetate (3 x 10 ml). The combined organics were dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography (eluant: hexane: ethyl acetate) then proceeded to provide the desired compound.l-(4-(2-(4-Chlorophenoxy)phenylamino)-2-phenylpiperidin-l-yl)ethanone STX2419C25H25ClN2O2, MoI. Wt.: 420.93Yellow oil, 41.3 mg, 21%1H NMR: (CDCl3, 270 MHz): delta 1.55-1.76 (2H, m, 2 x CH), 2.10 (1.5H, s, CH3), 2.23 (1.5H3 s, CH3), 2.69-2.82 (2H, m, CH), 3.12-3.22 (0.5H, m, CH)3 3.37-3.48 (0.5H5 m,CH), 3.52-3.62 (0.5H, m, CH), 3.75 (0.5H, ‘d’, J- 14.1 Hz, CH), 3.87-4.02 (0.5H, br S3CH), 4.74 (0.5H3 ‘d J = 13.9 Hz3 CH)3 5.17-5.23 (0.5H3 m, CH)3 6.13-6.14 (0.5H3 m, EPO CH), 6.57-6.68 (2H, m, Ar-H), 6.79 (IH, d, J= 7.9 Hz, Ar-H), 6.87 (2H, d, J= 7.7 Hz, Ar-H), 7.00 (IH, eq J = 6.7, 13.9 Hz, Ar-H), 7.19-7.46 ppm (7H, m, Ar-H). 13C NMR (CDCl3, 67.93 MHz): delta 21.6, 21.8, 32.5, 33.5, 34.5, 36.2, 37.4, 42.0, 45.8, 45.9, 50.6, 56.2, 112.2, 112.3, 117.5, 118.8, 119.6, 125.3, 125.8, 126.1, 126.5, 127.6, 128.0, 129.0, 129.4, 129.8, 138.2, 138.8, 143.1, 156.1, 167.3 ppm.HPLC: 2.355 min, 96.2% purity, (isocratic, 90% acetonitrile : 10% water at 1.0 ml/min) LCMS: 1.623 min, (95% MeOH : 5% water at 1.0 ml/min), ES”: 419.42.

According to the analysis of related databases, 2770-11-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; STERIX LIMITED; WO2007/3934; (2007); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 1435-48-9, 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. 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(5) Dissolving 35 g (0.1 mol) of the hydrochloride salt of Compound C in DMF 1000 mL in a reaction flask.Further add 2,4-dichlorofluorobenzene: 18g (0.11mol), add 27.5g (0.2mol) of potassium carbonate and 3.3g (0.02mol) of potassium iodide, and heat to reflux. After the reaction is complete, add 500mL of ammonia water and stir at room temperature. After 1 h, filtration, the filter cake was washed with 175 g of isopropyl alcohol and 70 g of methanol, and dried under vacuum at 60 C to a constant weight to obtain a beige powdery solid gefitinib 40 g, yield 91%.

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, 2,4-Dichloro-1-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jinan Ai Si Pharmaceutical Technology Co., Ltd.; Peng Lizeng; Wang Jianhua; Li Dongmei; Ji Songtao; (15 pag.)CN108503597; (2018); A;,
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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. 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 1-tert-Butyl-4-chlorobenzene

1000 g (5.93 mol) of 4-tert-butylchlorobenzene was dissolved in 250 g of 1,2-dichloroethane.A 4-tert-butylchlorobenzene solution was prepared.2000 g (20 mol) of 95%-98% sulfuric acid was added dropwise to 643 g (10 mol) of 95%-98% nitric acid dissolved in a 2 liter three-necked flask kept in an ice water bath to prepare a mixed acid of nitric acid sulfuric acid. .First nitrification reaction:According to the molar ratio of 4-tert-butylchlorobenzene to nitric acid 1:1.2, the reaction temperature is 60-80 C, the flow rate of 4-tert-butylchlorobenzene is 2.5 mL/min, the mixed acid flow rate is 2.6 mL/min, part of 4-un The mixed acid of the butylchlorobenzene solution and the nitric acid sulfuric acid is pumped through the continuous flow microreactor, which comprises a separate fluid module connected in sequence, specifically an inlet mixing reaction module,8 resident modules and one exit module, as described above.Each individual fluid module was maintained at a constant reaction temperature with a reaction residence time of 164 s.The nitration mixture obtained by the reaction is passed through a water separator to separate the first spent acid and the first nitration mixture.

The synthetic route of 3972-56-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shandong Heroic Chemical Co., Ltd.; Wang Yuanchao; Li Rixiang; Yang Anming; Lu Xiao; Ren Miaomiao; Zhang Yingjie; (19 pag.)CN109970566; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 210532-25-5,Some common heterocyclic compound, 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, molecular formula is C6H3ClF2O2S, 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 suspension of 3-amino-4,5,6,7-tetrahydro-pyrazolo[4,3-c]pyridine-2-carboxylic acid ethyl ester hydrochloride (36.2 g, 127.8 mmol) in anhydrous dichloromethane (1 L), at 0-5C, N,N-diisopropylethylamine (111.3 mL, 639 mmol) was added. To the resulting solution, 3,5-difluorobenzenesulfonyl chloride (27.17 g, 127.8 mmol) was added portionwise. The mixture was stirred at 0-5C for 1 hour then at room temperature for 3 hours. The organic phase was washed with NaHCC>3 satured solution, water and brine, dried over sodium sulfate filtered and evaporated. The crude, was triturated with diethylether (500 mL) to obtain the title compound as yellowish solid (45.48 g, 92%). IH-NMR (400 MHz), delta (ppm, DMSOtZ6): 7.71 (m, IH), 7.51 (m, 2H), 6.38 (bs, 2H), 4.34 (q, J=7.1 Hz, 2H), 3.99 (s, 2H), 3.44 (m, 2H), 2.58 (m, 2H), 1.30 (t, J= 7.1 Hz, 3H).

The synthetic route of 210532-25-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NERVIANO MEDICAL SCIENCES S.r.l.; WO2007/68619; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 13726-14-2, 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. 13726-14-2, name is 4-Chloro-3-methoxyaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of 2 (100 mg, 0.411 mmol), aniline (154 mg, 0.411 mmol) and DIPEA (0.15 mL, 0.822 mmol) in n-butanol (20 mL) were added, and the mixture was stirred at 110 C for 12 h. After cooling to room temperature, the reaction mixture was concentrated. The residue was purified by silica gel chromatography using a polarity mobile phase (acetone/dichloromethane, 10:100) to give product 3a.

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

Reference:
Article; Bertrand, Jeanluc; Castro, Alejandro; Dostalova, Hana; Espinosa-Bustos, Christian; Jorda, Radek; Krystof, Vladimir; Maria Zarate, Ana; Mella, Jaime; Salas, Cristian O.; Bioorganic Chemistry; (2019);,
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. 933190-51-3, name is 8-Bromo-6-chloroimidazo[1,2-b]pyridazine, A new synthetic method of this compound is introduced below., Product Details of 933190-51-3

To a solution of 6-fluoropyridin-2-amine (1.12 g, 10 mmol) in DMF (16 mL) was added NaH (0.24 g, 60% dispersion in mineral oil, 10 mmol) and the mixture stirred for 0.5 h. To the mixture was added 6-chloro-N-(6-fluoropyridin-2-yl)imidazo[1,2-b]pyridazin-8-amine (0.93 g, 4 mmol) under N2. The mixture was stirred at room temperature for 16 h, then partitioned between 45 mL of saturated NH4Cl solution and 45 mL of ether. The organic layer was washed with water (30 mL×3) and saturated NaCl solution (30 mL×3), dried over Na2SO4, concentrated in vacuo, and purified by chromatography (silica gel, 200-300 mesh, petroleum ether:ethyl acetate=3:1) to give 6-chloro-N-(6-fluoropyridin-2-yl)imidazo[1,2-b]pyridazin-8-amine (1.04 g, 99%) as a light brown solid. LC-MS: [M+H]+, 264.1, 266.2, tR=1.601 min.

The synthetic route of 933190-51-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; Hermann, Johannes Cornelius; Kuglstatter, Andreas; Lucas, Matthew C.; Padilla, Fernando; Wanner, Jutta; Zhang, Xiaohu; US2013/109661; (2013); A1;,
Chloride – Wikipedia,
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Synthetic Route of 2770-11-8,Some common heterocyclic compound, 2770-11-8, name is 2-(4-Chlorophenoxy)aniline, molecular formula is C12H10ClNO, 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.

2-(4-Chlorophenoxy)aniline (137 mg, 0.6237 mmol, 1.1 eq) and l-acetyl-N-(3- acetylphenyl)piperidine-4-carboxamide (160 mg, 0.5549 mmol, 1 eq) were stirred in dry dichloromethane (DCM) at room temperature for 10 min. Tri-isopropoxytitanium chloride (295 muL, 1.2351 mmol, 2.2 eq) was added to the reaction mixture which was stirred at room temperature for an additional 10 min. Sodium triacetoxyborohydride (590 mg, 2.7838 mmol, 5 eq) and acetic acid (3 drops) were added to the reaction mixture which was stirred at room temperature for 16 h. The reaction mixture was then poured onto a solution of saturated aqueous sodium bicarbonate (100 mL) and extracted with DCM (80 mL). The organic layer was washed with brine (100 mL), dried over MgSO4, filtered and concentrated to give the crude as a yellow oil. Purification of the crude by flash chromatography (ISCO) eluting with a gradient [from 100% petroleum ether (PE) to 100% EtOAc] gave the title compound (48 mg, 18%) as a clear oil.1R NMR (270 MHz, CDCl3) delta 1.43 (3H, d, J = 7.0 Hz, CH3), 1.60-1.95 (4H, m, 2chiCH2), 2.07 (3H, s, CH3), 2.38-2.52 (IH, m, CH), 2.55-2.72 (2H, m, CH2), 3.01-3.15 (2H, m, CH2), 4.36-4.50 (2H, m, CH + NH), 6.40-6.48 (IH, m, ArH), 6.52-6.60 (IH, m, ArH), 6.75-6.95 (4H, m, ArH), 7.04-7.09 (IH, m, ArH), 7.19-7.28 (3H, m, ArH), 7.35-7.50 (2H, m, ArH), 7.78 (IH, br s, NH); 13C NMR (67.5 MHz, CDCl3) delta 21.6, 25.2, 41.0, 45.8, 53.3, 60.5, 113.0, 117.0, 117.1, 118.6, 118.8, 119.2, 119.4, 119.6, 125.3, 129.4, 129.7, 138.4, 139.4, 142.6, 146.4, 156.3, 169.1, 172.5; LCMS (90% MeOH and 10% H2O;Symmetry C18 reverse phase column) ttau = 2.32 min; (ES”), m/z 492 ( ?3″5C, lM”, 75%), 494 (37ClM”, 25%); HRMS (ESI) calcd. for C28H31ClN3O3 (M+H)+ 492.2048, found 492.2051.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(4-Chlorophenoxy)aniline, its application will become more common.

Reference:
Patent; STERIX LIMITED; WO2009/66072; (2009); A2;,
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. 108-37-2, name is 1-Bromo-3-chlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C6H4BrCl

To a solution of diisopropylamine (76 mL, 0.4 mol) in anhydrous THF (664 mL) and n-hexane (220 mL) was added 2.5 M n-BuLi (160 mL, 0.4 mol) dropwise at -78 C. over 1 h. The mixture was stirred for 1 h at -78 C. and a solution of 1-bromo-3-chlorobenzene (76 g, 0.4 mol) in anhydrous THF (300 mL) was added dropwise at -78 C. After stirring for an additional 1 h at the same temperature, a solution of iodine (101 g, 0.4 mol) in anhydrous THF (400 mL) was added dropwise at -78 C. The temperature was raised from -78 C. to rt during 2 h. After stirring for 18 h at rt, the mixture was concentrated in vacuo to give the crude product (120 g) which was distilled under reduced pressure to give 1-bromo-3-fluoro-2-iodobenzene (115 g, 91%). 1H NMR (400 MHz, CDCl3) delta ppm 7.12-7.18 (t, 1H), 7.35-7.41 (dd, 1H), 7.49-7.54 (dd, 1H); MS (E/Z): 317 (M+H+)

According to the analysis of related databases, 108-37-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Baldwin, John J.; Cacatian, Salvacion; Claremon, David; Dillard, Lawrence W.; Flaherty, Patrick T.; Ghavimi-Alagha, Bahman; Ghirlanda, Damiano; Ishchenko, Alexey V.; Kallander, Lara S.; Lawhorn, Brian; Lu, Qing; McGeehan, Gerard; Knapp-Reid, Beth A.; Semus, Simon; Simpson, Robert D.; Singh, Suresh B.; Terrell, Lamont R.; Tice, Colin; Tran, Tritin; Xu, Zherong; Yuan, Jing; Zhao, Wei; Zhao, Yongdong Y.; US2010/317697; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics