Month: August 2021

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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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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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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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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Application of 2106-02-7, A common heterocyclic compound, 2106-02-7, name is 2-Chloro-4-fluoroaniline, molecular formula is C6H5ClFN, 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: General procedure for synthesis of various 7-chloroquinolin-4-yl-phenylamine (1a-1p) Compounds were synthesized using 4, 7-dichloroquinoline and suitable substituted anilines. Briefly, equimolar quantities of anilines (1 mmol) and 4, 7-dichloroquinoline (1 mmol) were refluxed in dry ethanol in basic medium (1.2 mmol K2CO3) for 2-16 h depending upon the various substituents. Progress of reaction was monitored by thin layer chromatography. After completion of reaction, reaction mixture was neutralized by 1 N NaOH solution and extracted with 3 * 50 mL of CHCl3, washed with NaHCO3 and brine. The organic layer was dried over anhydrous Na2SO4. The solvent was again evaporated under reduced pressure. The ligands were purified by successive recrystallization [32].

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; Singh, Shailja; Agarwal, Drishti; Sharma, Kumkum; Sharma, Manish; Nielsen, Morten A.; Alifrangis, Michael; Singh, Ashok K.; Gupta, Rinkoo D.; Awasthi, Satish K.; European Journal of Medicinal Chemistry; vol. 122; (2016); p. 394 – 407;,
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Related Products of 26487-67-2, The chemical industry reduces the impact on the environment during synthesis 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, I believe this compound will play a more active role in future production and life.

0.12 g (3 mmol) of a 60percent NaH suspension in mineral oil were added under nitrogen to a solution of pyrazolo[1,5-a]pyridin-2-ylmethanol (100 mg, 0.67 mmol) in 5 mL of dry THF. The mixture was stirred for 5 h at room temperature, and after this time, was added 1-(2-chloroethyl)azepane hydrochloride (201 mg, 1.01 mmol) suspended in 8 mL of THF with 200mul of triethylamine (TEA). The mixture was heated at 55 ºC for 18 h, allowed to cool to room temperature, quenched with water and extracted with EtOAc, and washed with water. The organic layers were dried over Na2SO4 and concentrated under vacuum to afford 0.22 g (65percent) of brown oil.

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-Chloroethyl)azepane hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Laboratorios del. Dr. Esteve, S.A.; Diaz-Fernandez,Jose-Luis; Cuberes-Altisent,Mª Rosa; EP2631236; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 433-94-3,Some common heterocyclic compound, 433-94-3, name is 2-Chloro-6-(trifluoromethyl)aniline, molecular formula is C7H5ClF3N, 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.

First, 30 g (0.153 mol) 2-chloro-6-trifluoromethylaniline (commercially available)765 ml of dimethyl sub-grind (DMSO)Followed by the addition of 68.1 g (0.23 mol) of 2-iodoheptafluoropropane,46 ml 1 molar aqueous solution of iron (II) sulfate with 15.4 g 98% strength sulfuric acid.The mixture was then degassed with argon,And using a syringe pump,Then 34.8 g of a 30% strength aqueous hydrogen peroxide solution was added dropwise over 30 minutes.During the addition,The temperature rose to 70 C.The mixture was allowed to stir for another 20 minutes,During that period,The temperature dropped to 30 C.The reaction mixture was then poured onto a saturated aqueous solution of sodium hydrogencarbonate,And extracted with ethyl acetate.The combined extracts were washed with water,Followed by washing with a saturated aqueous solution of sodium hydrogen sulfate and a saturated aqueous solution of sodium chloride,Dried over sodium sulfate,And concentrated on a rotary evaporator under reduced pressure. In terms of purification,The residue was placed in cassettes containing 330 g of silica gel,Gradient chromatography using pure cyclohexane to 90:10 (v / v) cyclohexyl acetate / ethyl acetate. This gave 46.1 g of 2-chloro-4-heptafluoroisopropyl-6-trifluoromethylaniline.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-6-(trifluoromethyl)aniline, its application will become more common.

Reference:
Patent; BAYER CROPSCIENCE AKTIENGESELLSCHAFT; HALLENBACH, WERNER; SCHWARZ, HANS-GEORG; GOERGENS, ULRICH; ILG, KERSTIN; TURBERG, ANDREAS; HORSTMANN, SEBASTIAN; KOEHLER, ADELINE; (178 pag.)TW2016/7938; (2016); A;,
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Reference of 932-96-7, 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 932-96-7 as follows.

General procedure:To a solution of 3-(chlorosulfonyl)benzoic acid (1.0 equiv, ca. 0.1 M) in dichloromethane, 4-bromo-N-methylaniline (3.1 equiv) was slowly added at 0 C with stirring. The mixture was stirred at room temp for 12 h. The solvent was removed with a nitrogen gas stream, the mixture was treated with 1 M NaOH (> 10 equiv), and was extracted with ether three times. The aqueous fraction was then acidified with 3 M HCl to pH ~1. The mixture turned cloudy during the addition. The resulting precipitate was collected by suction filtration on a Buchner funnel, washed with distilled water, and dried overnight at reduced pressure to give 3-(N-(4-bromophenyl)-N-methylsulfamoyl)benzoic acid (7a, 50-60%), which was used without further purification. To a solution of 7a (1.0 equiv, ca. 0.1 M), was added 4-chloro-N-methylaniline (1.1 equiv), EDCI (1.3 equiv), and DMAP (0.1 equiv). The mixture was stirred at room temp for 12 h and then diluted with excess EtOAc. The organic mixture was washed with 1 M aqueous HCl (2 times), 1 M aqueous NaHCO3 (2 times), and brine. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo to yield a crude product, which was purified by silica gel column chromatography to give 3a as a thick gel.

According to the analysis of related databases, 932-96-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Choi, Soo Hyuk; Quinti, Luisa; Kazantsev, Aleksey G.; Silverman, Richard B.; Bioorganic and Medicinal Chemistry Letters; vol. 22; 8; (2012); p. 2789 – 2793;,
Chloride – Wikipedia,
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Reference of 2533-69-9, The chemical industry reduces the impact on the environment during synthesis 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, I believe this compound will play a more active role in future production and life.

General procedure: Preparation of 2-methyl-6-nitro-2H-indazole (5d). To a stirred mixture of 6-nitro-1H-indazole (1.0 g, 0.0061 mmol) in dichloromethane (25.0 mL) was added trifluoromethanesulfonic acid (0.54 mL, 0.0061 mmol), stirred for 5-10 min at 25-35 C. To this mixture was added methyl 2,2,2,-trichlroacetimidate (2.69 g, 0.015 mmol) at room temperature. The reaction mixture was stirred at room temperature for 16-18 h under N2. After reaction completion, chilled saturated NaHCO3 solution was added. The aqueous and organic phases were separated. Aqueous phase was extracted with dichloromethane 10 mL. Combined organic layers were washed with DM water (2 × 10 mL). Organic layer was dried over anhydrous Na2SO4, filtered, and evaporated completely under vacuum to obtain 2-methyl-6-nitro-2H-indazole (1.03 g, 95.0%) as a yellow solid.

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, Methyl 2,2,2-trichloroacetimidate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Baddam, Sudhakar Reddy; Uday Kumar; Panasa Reddy; Bandichhor, Rakeshwar; Tetrahedron Letters; vol. 54; 13; (2013); p. 1661 – 1663;,
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108649-59-8, name is 1-(2-Bromoethyl)-2,4-dichlorobenzene, 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. Quality Control of 1-(2-Bromoethyl)-2,4-dichlorobenzene

General procedure: Pyridine or 4-picoline (1 mmol) and phenylalkyl halide derivatives (1.2 mmol) were condensed at 140 C to yield the corresponding N-phenylalkyl pyridinium halides.refPreviewPlaceHolder26 W. Wichitnithad, T.J. McManus and P.S. Callery. Rapid Commun. Mass Spectrom., 24 (2010), p. 2547. [26] and refPreviewPlaceHolder[47] The products were solidified from diethyl ether. Sodium borohydride (5 mmol) was added in portions to a stirred solution of the N-phenylalkyl pyridinium halide (1 mmol) in 30 mL of dry methanol at 0 C. The mixture was stirred for an additional 4 h, and the solvent was subsequently removed under reduced pressure. The residue in 30 mL of water was extracted with ethyl acetate (3 × 20 mL). The combined organic layers were dried (MgSO4), filtered, and concentrated to near dryness under reduced pressure. The crude tetrahydropyridine was purified by column chromatography on silica using 1% triethylamine in hexane/ethyl acetate (1:5). The obtained product was eluted through a basic alumina column with CH2Cl2 to yield the corresponding N-phenylalkyl substituted 1,2,3,6-tetrahydro-pyridine, which was converted to the hydrochloride salt by dissolving the free base in 10 mL of 120 mM ethanolic HCl and evaporating to afford pure tetrahydropyridine hydrochloride.

The synthetic route of 108649-59-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wichitnithad, Wisut; O’Callaghan, James P.; Miller, Diane B.; Train, Brian C.; Callery, Patrick S.; Bioorganic and Medicinal Chemistry; vol. 19; 24; (2011); p. 7482 – 7492;,
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