Category: chlorides-buliding-blocks

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. 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2,4-Dimethoxybenzene-1-sulfonyl chloride

A solution of 1.64 g of the compound obtained in the preceding step in 20 ml of DMF is cooled to 4 C., 0.25 g of 60% sodium hydride in oil is added and the mixture is stirred at 4 C. for 30 minutes. 1.34 g of 2,4-dimethoxybenzenesulphonyl chloride are then added and the mixture is stirred at RT for 4 hours. 50 ml of water are added to the reaction mixture, the resulting mixture is extracted with EtOAc, the organic phase is washed with saturated NaCl solution and dried over Na2SO4, and the solvent is evaporated off under vacuum. The residue is chromatographed on silica gel, eluting with a DCM/EtOAc mixture (97/3; v/v). 2 g of the expected product are obtained after crystallization from a DCM/iso ether mixture.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 63624-28-2.

Reference:
Patent; Di Malta, Alain; Garcia, Georges; Roux, Richard; Schoentjes, Bruno; Serradeil-Le Gal, Claudine; Tonnerre, Bernard; Wagnon, Jean; US2004/180878; (2004); 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. 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene, A new synthetic method of this compound is introduced below., Safety of 2,4-Dichloro-1-fluorobenzene

2,4-dichlorofluorobenzene 165g (1mol) and Catalyst Cat.1 0.77g were added to the reaction flask.Warm up to 40 C,Further introducing CO2 to 2 MPa, and stirring the reaction for 3 hours to obtain a reaction liquid;Further, 15.4 g (0.1 mol) of CCl4 was added dropwise to the reaction liquid, and the temperature was raised to 60 C.Insulation reaction for 2 hours,The hydrogen chloride formed by the reaction is absorbed by the falling film, and after the reaction is completed,The material obtained by the reaction is filtered to recover Catalyst Cat.1, and the filtrate is distilled under reduced pressure.2,4-dichloro-5-fluorobenzoyl chloride 44.95g,The yield was 98.8%.

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; Zhejiang Ben Li Technology Co., Ltd.; Gu Haining; Wu Zhengjie; Yu Yongzhi; Xu Hongshun; (10 pag.)CN109553524; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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 2533-69-9, Product Details of 2533-69-9

Put the compound (1,2-phenylenediamine) (2 g, 10 mmol) shown in Formula 3 at room temperature,Add acetic acid (20mL) to the reaction flask, cool in an ice bath, and slowly add the compound shown in Formula 1 (2,2,2-trichloroimino to methyl acetate) (1.3mL, 10mmol) as the starting material.After the addition was complete, the mixture was stirred at room temperature for 1 hour. TLC showed that the reaction was complete.Saturated sodium bicarbonate solution neutralized excess acid, extracted with ethyl acetate,Dry over anhydrous sodium sulfate, filter,Concentration gave the compound (2-trichloromethyl-benzopyrimidine) represented by Formula 3 (2.6 g, 60%).

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

Reference:
Patent; Sun Yat-sen University; Fu Jiasheng; Lu Paxiama; G .leikexima Leidi; Hu Wenhao; Wang Xin; Huang Jiawu; Lin Zebin; (22 pag.)CN110606850; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 873-38-1, These common heterocyclic compound, 873-38-1, name is 2-Bromo-4-chloroaniline, 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 suspension of 2-bromo-4-chloroaniline (5g, 24.22 mmol) in HCl (36.5%wt, 30 mL, 365 mmol) and water (100 mL) at -5C, a solution of sodium nitrite (1.838 g, 26.6 mmol) in water (10 mL) was added dropwise. The mixture was stirred at -5C for 1 h, and the suspension turn into a clear solution. A solution of sodium azide (1.732 g, 26.6 mmol) in water (10 mL) was added dropwise to the reaction. Solids precipitated out from the solution during the addition. It was stirred at -5C for 0.5 h. The mixture was extracted with ethyl acetate (70 mL x 3). The combined organic layers were washed with saturated aqueous sodium bicarbonate (20 mL), water (40 mL) and brine (50 mL) sequentially. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give the title compound.

The synthetic route of 873-38-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; XU, Jiayi; ALI, Amjad; ZHOU, Wei; GAO, Ying-Duo; EDMONDSON, Scott, D.; MERTZ, Eric; NEELAMKAVIL, Santhosh, F.; LIU, Weiguo; SUN, Wanying; SHEN, Dong-Ming; HARPER, Bart; ZHU, Cheng; BARA, Thomas; LIM, Yeon-Hee; YANG, Meng; (227 pag.)WO2017/74832; (2017); 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. 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine, A new synthetic method of this compound is introduced below., Quality Control of 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine

To a suspension of 3,6-dichloro-[1,2,4]triazolo[4,3-b]pyridazine (0.5 g, 1.8 mmol), 4-fluoro-N-(2-methoxy-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-yl)benzenesulfonamide (0.8 g, 2.2 mmol) and Pd(dppf)Cl2.CH2Cl2 (0.15 g, 0.18 mmol) in DME (20 mL) was added a solution of Cs2CO3 (1.2 g, 3.6 mmol) in H2O (2 mL). The resulted mixture was stirred at 70 C. under N2 atmosphere for 12 hours and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (v/v)=1/2) to give the title compound as a pale yellow solid (0.5 g, 64%). MS (ESI, pos. ion) m/z: 435.0 [M+H]+; 1H NMR (400 MHz, CDCl3): delta 10.20 (s, 1H), 8.71 (d, J=2.2 Hz, 1H), 8.46 (d, J=9.8 Hz, 1H), 8.27 (d, J=2.2 Hz, 1H), 8.04 (d, J=9.8 Hz, 1H), 7.90-7.87 (m, 2H), 7.42-7.38 (m, 2H), 3.79 (s, 3H).

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; Calitor Sciences, LLC; Xi, Ning; US2014/134133; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 27139-97-5, 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. 27139-97-5, name is 2-Bromo-4-chloro-1-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

To a reaction vessel purged with nitrogen were charged 45 g of 2-bromo-4-chlorotoluene, 36.6 g of carbazole, 7.0 g of a copper powder, 90.8 g of potassium carbonate, 4.7 ml of dimethyl sulfoxide, and 25 ml of dodecylbenzene, followed by heating, and stirred at 200°C for 44 hours. After cooling to 80°C, thereto was added 400 ml of toluene, an insoluble matter was removed by filtration therefrom, and vacuum concentration was conducted to obtain a crude product. Hexane was added to the crude product to precipitate the crude product. It was collected by filtration and then purified by column chromatography (carrier: silica gel, eluent: hexane) to obtain 20.3 g (yield: 32percent) of 9-(3-chloro-6-methylphenyl)-9H-carbazole as a white powder.

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

Reference:
Patent; Hodogaya Chemical Co., Ltd.; Shinshu University; YOKOYAMA Norimasa; KABASAWA Naoaki; ICHIKAWA Musubu; OTSURU Sohei; EP2679587; (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. 4152-90-3, name is (3-Chlorophenyl)methanamine, A new synthetic method of this compound is introduced below., name: (3-Chlorophenyl)methanamine

5-[3-(3-Chloro-benzylamino)-phenyl]-5-methyl-5,6-dihydro-2H-[l,4]oxazin-3-ylamine a) (RS)- (3-Chloro-benzyl)-[3-(5-methoxy-3-methyl-3,6-dihydro-2H-[l,4]oxazin-3-yl)- phenyl] -amineA dried pressure tube was charged consecutively under a nitrogen atmosphere with a solution of (RS)-3-(3-bromo-phenyl)-5-methoxy-3-methyl-3,6-dihydro-2H [l,4]oxazine (150 mg, 0.5 mmol) in toluene (5 ml), sodium tert-butylate (157 mg, 1.6 mmol), 2-di-tert-butylphosphino-2′,4′,6′- triisopropylbiphenyl (ie/t-butyl-x-phos) (23 mg, 0.1 mmol), tris(dibenzylideneacetone)- dipalladium chloroform complex (17 mg), and 3-chlorobenzylamine (154 mg, 1.1 mmol). The sealed pressure tube was heated at 100 C for 15 hours. After cooling, the reaction mixture was evaporated to dryness and directly purified by chromatography on an Isolute flash NH2 column using a gradient of heptane/ethyl acetate = 100/0 to 50/50 as the eluent. 85 mg (47%) of (RS)- (3-chloro-benzyl)-[3-(5-methoxy-3-methyl-3,6-dihydro-2H-[l,4]oxazin-3-yl)-phenyl]-amine were obtained as a yellow oil. Mass (calculated) C19H21CIN2O2 [344.844]; (found) [M+H]+ = 345.

The synthetic route of 4152-90-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; SIENA BIOTECH S.P.A; ANDREINI, Matteo; GABELLIERI, Emanuele; GUBA, Wolfgang; HILPERT, Hans; MAUSER, Harald; MAYWEG, Alexander V.; NARQUIZIAN, Robert; POWER, Eoin; TRAVAGLI, Massimiliano; WOLTERING, Thomas; WOSTL, Wolfgang; WO2012/98064; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 14862-52-3, 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. 14862-52-3, name is 3,5-Dibromochlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of 1,3-dibromo-5-chlorobenzene (800 mg, 2.96 mmol) and 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (600 mg, 2.96 mmol) in 1,4-dioaxane (15 mL) K2CO3 (1.2 g, 8.80 mmol) was added and the mixture was degassed with argon for 20 minutes. Pd (PPh3)4 (102 mg, 0.08 mmol) was added to reaction mixture and degassed for another 20 minutes. The reaction mixture was refluxed under stirring for 8 hours and then filtered through celite pad. The filtrate was concentrated and the residue was purified by column chromatography on silica (100-200 mesh) eluting with 15% ethyl acetate in petroleum ether to afford the title compound as white solid (400 mg, 50 %). 1H NMR: (300 MHz, CDCl3) delta 8.70 (dd, J = 4.5, 1.5 Hz, 2H), 7.65-7.64 (m, 1H), 7.59-7.58 (m, 1H), 7.54-7.53 (m, 1H), 7.45 (dd, J = 4.2, 1.5 Hz, 2H); ESIMS: m/z = 268.0 [(M+H)+].

The synthetic route of 3,5-Dibromochlorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Blass, Benjamin E.; Iyer, Pravin; Abou-Gharbia, Magid; Childers, Wayne E.; Gordon, John C.; Ramanjulu, Mercy; Morton, George; Arumugam, Premkumar; Boruwa, Joshodeep; Ellingboe, John; Mitra, Sayan; Reddy Nimmareddy, Rajashekar; Paliwal, Shalini; Rajasekhar, Jamallamudi; Shivakumar, Savithiri; Srivastava, Pratima; Tangirala, Raghuram S.; Venkataramanaiah, Konda; Bobbala, Ramreddy; Yanamandra, Mahesh; Krishnakanth Reddy; Bioorganic and Medicinal Chemistry Letters; vol. 28; 13; (2018); p. 2270 – 2274;,
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 2106-04-9 as follows. HPLC of Formula: C6H5ClFN

Example 3; Step 1; A round bottom flask was charged with 1 eq of 3-chloro-2-fluoroaniline (3A), 1-methyl-2-pyrrolidinone (about 1.5 M 3A in NMP), 2.2 eq of sodium cyanide, and 1.35 eq of nickel(II) bromide at RT under N2. The concentration was halved by the introduction of additional NMP under N2 and the solution was gently warmed to 200+/-5 C. and stirred for 4 days under N2. The reaction mixture was allowed to cool to room temperature. The reaction mixture was diluted with 30 volumes of tert-butyl methyl ether (MTBE) and filtered through celite. The celite pad was then rinsed with 10 volumes of MTBE. The organics were washed with 40 volumes of brine, 2×40 volumes of water and 40 volumes of brine. The combined organics were dried over sodium sulfate and concentrated to afford a brown solid, which was dried under vacuum (-30 in Hg) at 40 C. for 8 hours to afford the compound of Formula 3B (71% yield).

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; Morgan, Bradley Paul; Muci, Alex; Lu, Pu-Ping; Kraynack, Erica Anne; Tochimoto, Todd; Morgans, David J.; US2006/14761; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 6775-78-6, name is 6-Chloroimidazo[1,2-b]pyridazine, 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. Computed Properties of C6H4ClN3

478 mg (3.1 1 mmol) of 6-chloroimidazo[1 ,2-b]pyridazine were introduced into 10 mL of chloroform under argon and, while cooling in ice, 664 mg (3.73 mmol) of N- bromosuccuinimide were added. After the addition was complete, the reaction mixture was stirred at room temperature overnight. The reaction mixture was then mixed with water and ethyl acetate and, after addition of saturated sodium bicarbonate solution, the phases were separated. The aqueous phase was extracted three more times with ethyl acetate. The combined organic phases were then washed with brine and dried over sodium sulfate. In the final removal of the solvent in vacuo, the desired product was isolated in quantitative yield in the form of an amorphous white solid which was employed without further chromatographic purification in subsequent reactions.

The synthetic route of 6-Chloroimidazo[1,2-b]pyridazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; EIS, Knut; PUeHLER, Florian; ZORN, Ludwig; SCHULZE, Volker; SUeLZLE, Detlev; LIENAU, Philip; HAeGEBARTH, Andrea; PETERSEN, Kirstin; BOeMER, Ulf; WO2013/149909; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics