Month: May 2021

Related Products of 6579-54-0, 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. 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

a) 2-{[(2-Morpholin-4-yl ethyl)carbamoyl]amino}-1,3-benzothiazol-6-yl 2,6-dichlorobenzenesulfonate may be prepared in the following manner:To a solution of 260 mg of 1-(6-hydroxy-1,3-benzothiazol-2-yl)-3-(2-morpholin-4-ylethyl)urea in 19.4 cm3 of aqueous 0.1N sodium hydroxide solution are added 209 mg of finely ground 2,6-dichlorobenzenesulfonyl chloride. After stirring for about 5 hours at a temperature in the region of 20 C., a further 70 mg of 2,6-dichlorobenzenesulfonyl chloride are added. After stirring for about 18 hours at the same temperature, the reaction mixture is concentrated under reduced pressure (13 kPa) to a volume of about 5 cm3. The suspension obtained is cooled for about one hour at a temperature in the region of 5 C. The solid is filtered off by suction, washed with three times 2 cm3 of water precooled to about 5 C., and dried under reduced pressure (13 kPa) over phosphorus pentoxide. 216 mg of 2-{[(2-morpholin-4-ylethyl)carbamoyl]amino}-1,3-benzothiazol-6-yl 2,6-dichlorobenzenesulfonate are thus obtained in the form of a cream-coloured powder, the characteristics of which are as follows:Melting point: melting at 130 to 135 C. (Koefler block)1H NMR spectrum at 300 MHz: from 2.33 to 2.47 (m, 6H); from 3.22 to 3.38 (masked m, 2H); 3.59 (m, 4H); 6.79 (broad t, J=5.5 Hz, 1H); 7.01 (dd, J=2.5 and 9.0 Hz, 1H); 7.56 (d, J=9.0 Hz, 1H); from 7.69 to 7.81 (m, 4H); 10.95 (broad m, 1H)Mass spectrum: LCMS: m/z 531: [M+H]+, m/z 529: [M-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, 2,6-Dichlorobenzenesulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AVENTIS PHARMA S.A.; US2008/194555; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 95-51-2, The chemical industry reduces the impact on the environment during synthesis 95-51-2, name is 2-Chloroaniline, I believe this compound will play a more active role in future production and life.

General procedure: Into a pressure microreactor of stainless steel of 17 mL capacity or into a glass ampule (20 mL) (results of the parallel runs were virtually identic) was charged 5-10 wt % of catalyst (0.94HY-BS, NaY-BS, 0.72KNaX-BS), 100 mmol of aniline or its derivative, and 400 mmol of dimethyl carbonate. The reactor was hermetically closed (the ampule was sealed), and was heated for 1-4 h at 150 C. After the end of the run the reactor was cooled to room temperature, opened, the reaction mixture was filtered through a bed of Al2O3. Dimethyl carbonate was distilled off, the residue was distilled at atmospheric pressure or in a vacuum, or crystallized from ethanol.

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

Reference:
Article; Khusnutdinov; Shchadneva; Mayakova, Yu. Yu.; Ardieva; Khazipova; Kutepov; Russian Journal of Organic Chemistry; vol. 52; 11; (2016); p. 1565 – 1570; Zh. Org. Khim.; vol. 52; 11; (2016); p. 1574 – 1578,5;,
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. 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, A new synthetic method of this compound is introduced below., Application In Synthesis of 5-Chloro-1H-benzo[d][1,2,3]triazole

a. To a solution of 5-chloro-1H-benzotriazole (1 g) and sodium acetate (1 g) in acetic acid was added bromine (2 g). After 10 days at room temperature, the mixture was treated with a saturated solution sodium thiosulfate, neutralized with a saturated solution of sodium bicarbonate and extracted with ethyl acetate. The organic phase was washed with brine, dried over anhydrous sodium sulfate, filtered and the filtrate concentrated under reduced pressure to afford a residue that was purified by semi-preparative liquid chromatography to afford 4-bromo-5-chloro-1H-benzotriazole as an off-white solid (213 mg, 14%). MS (ES): M/Z [M+H]=232. 1H NMR: (400 MHz, DMSO-d6): 7.58 (d, J=8.7Hz, 2H) and 7.91 (d, J=8.7Hz, 1H).

The synthetic route of 94-97-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AVENTIS AGRICULTURE; MERIAL LIMITED; Soll, Mark David; Le Hir de Fallois, Loic Patrick; Huber, Scot Kevin; Lee, Hyoung Ik; Wilkinson, Douglas Edward; Jacobs, Robert Toms; US2014/80862; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 2687-12-9, name is Cinnamyl chloride, 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. Application In Synthesis of Cinnamyl chloride

EXAMPLE 1 Obtaining 2-(3-N,N-diisopropylamine-1-phenylpropyl)-4-carboxyphenol (IV’a) Diisopropylamine (2.77 1, 19.65 mol) and sodium iodide (16.95 g, 0.13 mol) were loaded onto a solution of cinnamyl chloride (1 kg, 6.55 mol) in ethanol (3 1/kg) at 20/25C. The mixture was heated at internal 80-85C, the reaction conditions being maintained for 3-4 hours until the end of such reaction. The mixture was cooled at 40-45C and distilled to an internal volume of 1.3 1. The mixture was then cooled at 20-25C, water (4 1) and toluene (3 1) was added and the pH was adjusted to 1.0-1.5. The phases were decanted and dichloromethane (4 1) was loaded onto the aqueous phase, adjusting the pH again to 11.5-12.0. The phases were decanted and the organic phase was washed with water (4 1). Once the phases were decanted, the organic phase was distilled at atmospheric pressure to an internal volume of 1.3 1 in order to then load heptane (0.5 1). Again, it was distilled to 1.3 1 and heptane (2 1) was loaded. The suspension which was obtained was filtered by a prelayer, which was washed with heptane (0.5 1). The filtered organic phase was distilled at atmospheric pressure to an internal volume of 1.3 1. The amine content of the reaction mixture was determined by the potentiometric titration thereof. Acetic acid (1.2 l/kg of amine), 4-hydroxybenzoic acid (0.63 kg/kg of amine, 1 equivalent), and, then, sulfuric acid (1.1 l/kg of amine, 4.5 equivalents) were loaded onto the mixture. It was heated at internal 80-85C, the reaction conditions being maintained for 5-6 hours until the end of the reaction. The reaction mixture was cooled to 35-40C and water (10 l/kg of amine) and ethyl acetate (10 l/kg of amine) were loaded. The phases were decanted and the organic phase was washed out with water (5 l/kg). The aqueous phases were pooled; toluene (5 l/kg of amine) was loaded, the phases were decanted and n-butanol (10 l/kg of amine) was loaded onto the aqueous phase, the pH was adjusted to 7 and it was decanted. The organic phase was distilled to an internal amine volume of 1.5-2.0 l/kg and then heptane (8 l/kg of amine) was loaded. The product which crystallized was cooled at 5-10C, filtered and washed with heptane (5 l/kg of amine). The product was then dried in an oven with air circulation for 10-12 hours, obtaining a product with an overall molar yield of 40% and with a purity greater than 90%. NMR (1H) DMSO: H8: doublet 0.8-0.9 ppm 12H, H5: multiplet 2.0-2.1 ppm 2H, H6: multiplet 2.3 ppm 2H, H7: multiplet 2.8-3.0 ppm 2H, H4: triplet 4.3 ppm 1H, H1: doublet 6.8 ppm 1H, H11: multiplet 7.1 ppm 1H, H10-9: multiplet 7.1-7.3 ppm 4H, H2: doublet 7.5 ppm 1H, H3: singlet 7.8 ppm 1H. NMR(13C) DMSO: 20.52; 20.57; 30.74; 36.11; 39.72; 48.04; 114.35; 125.56; 126.43; 128.59; 128.68; 129.02; 129.47; 129.77, 145.34; 157.76; 169.90.

The synthetic route of Cinnamyl chloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ragactives, S.L.U.; EP2281801; (2011); A1;,
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 61881-19-4 as follows. Computed Properties of C8H5ClF3N

X4 – 4 (594 mg, 1 mmol), N – benzene three fluorine second grades acyl chloride (0.45 ml, 3 mmol, 3 eq) dissolved in 8 ml of acetone, in batches adding potassium carbonate (410 mg, 3 mmol, 3 eq), stirring at room temperature 1 hour (TLC detection consumption end), filtering, the filtrate turns on lathe does, column to obtain white solid (601 mg, yield 79%)

According to the analysis of related databases, 61881-19-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Pharmaceutical Industry Institute; China Pharmaceutical Industry Zongyuan; Lin Feng; Lu Rui; Xu Qiulong; Chen Jianli; Han Jine; (33 pag.)CN104231009; (2017); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 367-22-6, A common heterocyclic compound, 367-22-6, name is 4-Chloro-3-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.

Iodine chloride (20.6 ml, 1M solution in DCM, 20.6 mmol) was added dropwise to a solution of 4-chloro-3-fluoroaniline (2 g, 13.7 mmol) in methanol (35 ml) at 0C and the reaction mixture was stirred for 1 h at room temperature. Volatiles were removed under reduced pressure, water was added and the mixture was extracted with dichloromethane. The combined organic layers were washed with water, dried with Na2S04 and evaporated. The remaining residue was purified by chromatography with three consecutive columns (silica gel, heptane/EtOAc 98:2 – 93:7 and twice heptane/EtOAc 98:2 – 95:5) to obtain the title compound (2.51 g, 67%) as dark red solid. MS (ESI): 272.1 (M+H)+.

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; F. HOFFMANN-LA ROCHE AG; CECCARELLI, Simona M.; CONTE, Aurelia; KUEHNE, Holger; KUHN, Bernd; NEIDHART, Werner; OBST SANDER, Ulrike; RUDOLPH, Markus; WO2013/64465; (2013); A1;,
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 57946-56-2 as follows. Formula: C6H5ClFN

General procedure: To a solution containing para-chloro-meta-fluoroaniline (10.0 g, 70.1 mmol) in 600 mL THF at 0 C was added Et3N (9.11 mL, 70.1 mmol) followed by ethyl oxalylchloride (7.70 mL, 70.1 mmol) dropwise over 15 minutes. The reaction mixture was warmed to room temperature and stirred for 18 hrs. The reaction mixture was filtered and the filter cake was washed with one-300 mL portion of ethyl acetate. The organic phase was washed with two-100 mL portions of 1M HCl, dried over MgSO4, filtered, and concentrated to give the product. Recrystallization from hot Et2O gave 14.4 g (84%) of 27 as a colorless crystalline solid.

According to the analysis of related databases, 57946-56-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Lalonde, Judith M.; Elban, Mark A.; Courter, Joel R.; Sugawara, Akihiro; Soeta, Takahiro; Madani, Navid; Princiotto, Amy M.; Kwon, Young Do; Kwong, Peter D.; Schoen, Arne; Freire, Ernesto; Sodroski, Joseph; Smith III, Amos B.; Bioorganic and Medicinal Chemistry; vol. 19; 1; (2011); p. 91 – 101;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 14862-52-3, 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. 14862-52-3, name is 3,5-Dibromochlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Toluene (200 ml) and water (50 ml)Of (9,9-dimethyl-9H-fluorene -2-yl) boronic acid (5.0 g, 21.0 mmol), 1,3-dibromo-5-chlorobenzene (14.19 g, 52.5 mmol), Pd (PPh3 ) it is refluxed in a solution of 4 (0.49 g, 0.42 mmol), and K2CO3 (5.80 g, 42.0 mmol) under nitrogen for 18 hours. After cooling to room temperature (~ 22 ), isolating the organic layer it was distilled off excess 1,3-dibromo-5-chlorobenzene. The residue as eluent heptane / DCM (9/1, v / v) for purification by column chromatography on silica gel, and as a colorless crystalline solid 2- (3-bromo-5-chlorophenyl) -9, 9-dimethyl -9H- FluoreneTo give a (6.2 g, 77%).

The chemical industry reduces the impact on the environment during synthesis 3,5-Dibromochlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Universal Display Corporation; Cheng, Licang; Rayekh, Suman; Vaudreuil, Pierre Ruik-T; Elshennawy, Zaineb; Kottas, Greg; Diatkine, Alexei Borysovych; Joseph, Scott; Adamowicz, Vadim; Xia, Chuanjun; Wang, Ting Chiu; Jage, Walter; (109 pag.)KR2016/6633; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 5013-77-4, name is N-Methyl-2,4-dichlorobenzylamine, 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 5013-77-4, Recommanded Product: N-Methyl-2,4-dichlorobenzylamine

Into a 250-mL 3-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 2-bromo-l-(4-bromophenyl)ethanone (9 3 g, 33 45 mmol, 1 00 equiv) in dioxane (100 mL), t?ethylamine (5 0 g, 1 50 equiv), and (2,4-dichlorophenyl)-N- methylmethanamine (64 g, 33 68 mmol, 1 00 equiv) The resulting solution was stirred for 2 h at 250C The solids were filtered out The filtrate was used for next step directly.

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; ARDELYX, INC.; CHARMOT, Dominique; JACOBS, Jeffrey, W.; LEADBETTER, Michael, Robert; NAVRE, Marc; CARRERAS, Chris; BELL, Noah; WO2010/78449; (2010); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 870-24-6,Some common heterocyclic compound, 870-24-6, name is 2-Chloroethanamine hydrochloride, molecular formula is C2H7Cl2N, 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: Benzenesulfonyl chloride(525 mg, * 380 lL, 3 mmoL) was gradually added to a50-mL round-bottom flask containing 2-chloroethylamine.HCl (116 mg, 3 mmol) in dimethyl formamide(5 mL) and triethylamine (TEA, 500 lL). The reaction mixture was stirred at room temperature for 3 h and then poured into a cold solution of HCl 5 % (50 mL). The precipitate was collected and dried under vacuum at 40C to give compound 2a, which was used for the next step without further purification.

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

Reference:
Article; Thuan, Nguyen Thi; Dung, Do Thi Mai; Que, Do Nguyet; Dung, Phan Thi Phuong; Vu, Tran Khac; Hahn, Hyunggu; Han, Byung Woo; Kim, Youngsoo; Han, Sang-Bae; Nam, Nguyen-Hai; Medicinal Chemistry Research; vol. 24; 11; (2015); p. 3803 – 3812;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics