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. 13526-66-4, name is 3-Bromo-6-chloroimidazo[1,2-b]pyridazine, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H3BrClN3

Intermediate P3-Bromo-6-(3-chlorophenoxy)imidazo[1,2-b]pyridazineVariant 3: 5 g (21.5 mmol) of 3-bromo-6-chloroimidazo[1,2-b]pyridazine, 3 g (23.7 mmol) of 3-chlorophenyl, 246 mg (0.27 mmol) of tris(dibenzylidineacetone)dipalladium, 500 mg of rac-BINAP and 4.1 g of sodium tert-butoxide are stirred in a mixture of 100 ml of dimethylformamide and 200 ml of tetrahydrofuran at 100 C. under a protective gas atmosphere for 12 h.The reaction mixture is then mixed with saturated sodium chloride solution. The aqueous phase is extracted with ethyl acetate. The organic phase is washed twice with dilute aqueous NaCl solution and once with saturated aqueous NaCl solution and dried over sodium sulfate. In the final purification by chromatography on silica gel, 2.78 g (40%) of the desired product were isolated.1H-NMR (DMSO-D6): delta=7.22 (d, 1H); 7.31-7.42 (m, 2H); 7.51 (d, 1H); 7.55 (t, 1H); 7.83 (s, 1H); 8.25 (d, 1H) ppm.MS (ESI): m/z=324/326 [M+H]+

According to the analysis of related databases, 13526-66-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PRIEN, Olaf; Eis, Knut; Bader, Benjamin; Guenther, Judith; Von Bonin, Arne; US2009/93475; (2009); 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. 2106-02-7, name is 2-Chloro-4-fluoroaniline, A new synthetic method of this compound is introduced below., name: 2-Chloro-4-fluoroaniline

Lithium hexamethyldisilazide (22.9 ml, 22.9 mmol, 1 M solution in tetrahydrofuran) wasadded over 5 mm to solution of 2-chloro-4-fluoroaniline (1 .84 g, 12.6 mmol, Gas No 2106-02-7) in tetrahydrofuran (60 ml) at -780 and the mixt ure was stired at -780 for 1 h. A solution of ethyl 4-{[tert-butyl(dimethyl)silyl]oxy}- 1 -(2-ch loroethyl)cyclohexanecarboxylate (mixture of cis-/trans-isomers) (4.00 g, 11 .5 mmol) in tetrahydrofuran (60 ml) was added and the mixture was stirred for 2 h at -780 and the for 3 days at room temperature. For work-up, the reactionmixture was poured into a mixture of water and saturated sodium bicarbonate solution, extracteted with ethyl acetate (3x) and the combined organic phases were washed with brine, filtrated through a silicone filter and concentrated under reduced pressured. The residue was purified by flash chromatography (Snap Gartdidge, hexanes/ethyl acetate gradient) to give 8-{[tert-butyl(dimethyl)silyl]oxy}-2-(2-chloro-4-fluorophenyl)-2-azaspiro[4.5]decan-1 -one in 2 fractions. Fraction 1 (1.88 g, isomer 1, conatains ca 2Omol%2-chloro-4-fluoroaniline) and fraction 2 (485 mg, isomer 2).

The synthetic route of 2106-02-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; EIS, Knut; ACKERMANN, Jens; WAGNER, Sarah; BUCHGRABER, Philipp; SUeLZLE, Detlev; HOLTON, Simon; BENDER, Eckhard; LI, Volkhart; LIU, Ningshu; SIEGEL, Franziska; LIENAU, Philip; BAIRLEIN, Michaela; VON NUSSBAUM, Franz; HERBERT,Simon; KOPPITZ, Marcus; (734 pag.)WO2016/177658; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 918538-05-3, 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. 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Synthesis of Compound 4.1. Into a 50-mL round-bottom flask, was placed 2,4- dichloropyrrolo[2, l- J[l,2,4]triazine (200 mg, 1.06 mmol, 1.00 equiv), sodium carbonate (227 mg, 2.14 mmol, 2.00 equiv), (r,4r)-Nl, ^-dimethyl cyclohexane-l,4-diamine (276 mg, 1.94 mmol, 1.20 equiv) in ACN (20 mL). The reaction was stirred overnight at 80 C in an oil bath. Then it was concentrated in vacuo and the residue was purified by silica gel column chromatography with dichloromethane/methanol (20: 1). This resulted in 180 mg (58%) of 4.1 as a white 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, 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NIMBUS IRIS, INC.; ROMERO, Donna; ROBINSON, Shaughnessy; GREENWOOD, Jeremy Robert; (102 pag.)WO2017/4134; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 118-69-4,Some common heterocyclic compound, 118-69-4, name is 2,6-Dichlorotoluene, molecular formula is C7H6Cl2, 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.

Ammoxidation runs were carried out in a fixed bed tubular quartz reactor, which is filled with 5g of catalyst particles prepared by the methods described in examples 1 to 3 and mixed with corundum particles of the same size in 1: 1 by weight ratio. A preheating zone is provided on the top of the catalyst bed. The catalyst was activated in a mixture of air and [NH3] at [400C] for 4 hours and then the catalytic runs were performed. The 2,6-DCT and [H20] were pumped in the mole ratio of 1: 15 to 20. The product stream was collected for every half-an-hour and analysed by gas chromatography. The reaction was carried out under the following reaction conditions. A reaction temperature of 350 to [400C] was used, and the GHSV comprised between 650-750 [H-‘.] The contact time consisted of 4.8 to 5.5 seconds. The mole ratio of 2,6-DCT : H20 : NH3: air was 1: 15: 3-4: 21, the molar concentration of 2,6-DCT was 2.4 % and the ratio of O/NH3 was 1. [1 %.]

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

Reference:
Patent; TESSENDERLO CHEMIE S.A.; WO2003/101939; (2003); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 3972-56-3,Some common heterocyclic compound, 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene, molecular formula is C10H13Cl, 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 sealable reaction tube equipped with a stirring bar was charged with PdCl2(CH3CN)2 (2.6 mg, 0.01 mmol), TIP-Cy*Phine (11.1 mg, 0.02 mmol), Cs2CO3 (652 mg, 2 mmol), 1-tert-butyl-4-chlorobenzene (169 mg, 1 mmol), phenylacetylene (123 mg, 1 mmol) and 2 mL of acetonitrile. The tube was then sealed with a Teflon-lined septum and heated to 90¡ã C. for 6 h with vigorous stirring. The resulting suspension was cooled to room temperature, diluted with EtOAc and filtered through a pad of Celite. The filtrate was concentrated in vacuo affording the crude product which was purified by flash chromatography on silica gel using hexanes as the eluent to give a pure white solid (213 mg, 91percent). 1H NMR (600 MHz, CDCl3) delta=7.54 (d, J=5.8 Hz, 2H), 7.49 (d, J=8.5 Hz, 2H), 7.37 (dd, J=21.8, 7.6 Hz, 5H), 1.35 (s, 9H). 13C NMR (151 MHz, CDCl3) delta=152.08, 132.13, 131.88, 128.86, 128.61, 125.90, 124.07, 120.79, 90.09, 89.28, 35.35, 31.75.

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

Reference:
Patent; Agency for Science, Technology and Research; Johannes, Charles W.; Robins, Edward G.; Jong, Howard; Lim, Yee Hwee; Chia, Saei Weng; Yang, Yong; Podichetty, Anil; (84 pag.)US2016/207034; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 7051-16-3, A common heterocyclic compound, 7051-16-3, name is 1-Chloro-3,5-dimethoxybenzene, molecular formula is C8H9ClO2, 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: In a microwave vial equipped with a stirring bar, potassium N-methyltrifluoroborate isoindolin-1-one (6) (80.1 mg, 0.316 mmol), potassium carbonate (104 mg, 0.752 mmol), Pd(MeCN)2Cl2 (4.9 mg, 7.5 mol%), and XPhos (17.9 mg, 15.0 mol%) were successively introduced. The vial was capped and put under inert atmosphere (3 x vacuum/N2 cycles). The electrophile was then introduced using a microsyringe (0.25 mmol, 1.0 equiv.) followed by 0.8 mL of degassed t-BuOH and 0.2 mL of degassed distilled water. The resulting mixture was then placed in an oil bath or a hotplate-magnetic stirrer system preheated at 100 C and stirred at this temperature overnight (reactions followed by thin-layer chromatography, TLC). After cooling to room temperature, the vial was uncapped and the reaction mixture was diluted with dichloromethane (DCM) (5 mL) and water (5 mL). The aqueous layer was extracted with dichloromethane (3 x 15 mL). Organic layers were combined, washed with brine solution, and dried over Na2SO4, and the solvent was removed under vacuum to yield the crude product. The crude product was purified by flash column chromatography on silica gel using 30% ethyl acetate/hexane as the eluent.

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; Nadaf, Rashid N.; Seapy, Dave G.; Synthetic Communications; vol. 44; 14; (2014); p. 2012 – 2020;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, molecular formula is C8H17Cl2N, 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. Recommanded Product: 26487-67-2

Compound 4 (200mg, 0.75mmol) refluxed with K2CO3 (259.42mg, 1.87mmol), 1-(2-Chloro-ethyl)-azepane hydrochloride (148.58mg, 0.75mmol) in acetone furnished 7 (220mg, 75percent) as brown viscous oil. 1H NMR (300MHz, CDCl3): delta 7.21?7.06 (m, 8H), 6.91?6.78 (m, 3H), 6.64?6.63 (m, 1H), 5.59 (s, 1H), 4.07 (t, J=6.0, 2H), 2.97 (t, J=6.1, 2H), 2.81 (t, J=5.6, 4H), 1.69?1.61 (m, 8H); 13C NMR (CDCl3, 50MHz): delta 157.5, 148.4, 144.1, 136.2, 129.8 (2C), 128.7 (2C), 128.4 (2C), 126.6, 126.5, 126.2, 124.4, 114.4 (2C), 65.7, 57.8, 54.9 (2C), 51.3, 25.7 (3C), 24.1; IR (Neat): 3019, 2938, 2362, 1610, 1509, 1218, 763cm?1; MS (ESI): m/z 392 (M+H)+; Anal. Calcd for C25H29NOS: C, 76.68; H, 7.46; N, 3.58. Found: C, 76.72; H, 7.39; N, 3.61.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 26487-67-2, its application will become more common.

Reference:
Article; Singh, Priyanka; Manna, Sudipta Kumar; Jana, Amit Kumar; Saha, Tiash; Mishra, Pankaj; Bera, Saurav; Parai, Maloy Kumar; Srinivas Lavanya Kumar; Mondal, Sankalan; Trivedi, Priyanka; Chaturvedi, Vinita; Singh, Shyam; Sinha, Sudhir; Panda, Gautam; European Journal of Medicinal Chemistry; vol. 95; (2015); p. 357 – 368;,
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. 1205-71-6, name is 4-Chloro-N-phenylaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1205-71-6

To a solution of 4-chloro-A/- phenylaniline 1 (0.2 g, 0.98 mmol) in dry DCM (3 mL) at 0 C was added triphosgene (0.32 g, 1 .08 mmol). Pyridine (0.1 1 mL, 1 .38 mmol) predissolved in 1 mL of DCM was added slowly to the reaction mixture. The reaction was stirred for another 15 min and then warmed to RT and stirred for 2 h. It was quenched under cooling by the slow addition of water (the solution turned pink). The mixture was extracted and the aqueous layer was washed again with DCM. The combined organic extracts were washed with brine, dried over MgS04, concentrated to give 0.24 g (92%) of the title compound as a peach colored solid. This was used in the next step without further purification. 1H NMR (400 MHz, Chloroform-d) d 7.47 – 7.27 (m, 9H).

According to the analysis of related databases, 1205-71-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF MICHIGAN; HOLINSTAT, Michael; ADILI, Reheman; WHITE, Andrew; (43 pag.)WO2019/204447; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 220227-21-4,Some common heterocyclic compound, 220227-21-4, name is 2,4,5-Trifluorobenzene-1-sulfonyl chloride, molecular formula is C6H2ClF3O2S, 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.

Synthesis of N-{5-[l-(2,4-Dichloro-benzyl)-5-fluoro-3-methyl-lH-indol-7-yl]- [l,3,4]oxadiazol-2-yl}-2,4,5-trifluoro-benzenesulfonamide, B12. A solution of 2,4,5-trifluorobenzenesulfonyl chloride (92 mg, 0.4 mmol, 4 equiv.) in pyridine (0.3 mL) was added to a mixture of 1-14 (39 mg, 0.1 mmol, 1 equiv.) and DMAP (49 mg, 0.4 mmol, 4 equiv.) at rt. The reaction mixture was heated to 90 0C for 2 h. The reaction mixture was then quenched with 10% aqueous HCl and extracted with ethyl acetate. The organic layer was washed with water, brine, dried over MgSO4, filtered, and concentrated in vacuo. The resulting oil was chromatographed on SiO2 (0.5 g), eluting with CH2Cl2 to afford B12 (10 mg, 17 %) as a yellow oil. Rf= 0.40 (EtOAc). 1H-NMR (400 MHz, CDCl3) 2.34 (d, J =1.2 Hz, 3H), 5.64 (s, 2H), 6.05 (d, J = 8.4 Hz, IH), 6.97 (dd, J = 8.4, 2.0 Hz, IH),7.03 (s, IH), 7.08 (m, IH), 7.29 (dd, J = 9.6, 2.4 Hz, IH), 7.35 (d, J = 2.0 Hz, IH), 7.51 (dd, J = 8.4, 2.4 Hz, IH), 7.86 (m, IH). LC-MS (95 %): ESI” Calcd. 586 (M) Found: 585.1 (M-I).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4,5-Trifluorobenzene-1-sulfonyl chloride, its application will become more common.

Reference:
Patent; DECODE CHEMISTRY, INC.; WO2006/44405; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, 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 14752-66-0, Recommanded Product: 14752-66-0

In a dry test tube, add 34mg and 198mg pyrazole of chlorobenzene sulfinateSodium, added 267mg of NBS. 2mL ethyl acetate was then added to dissolve the solid, the reaction solution was stirred at 25 12 hours. After completion of the reaction, ethyl acetate and water extraction, the resulting organic phase was concentrated on a rotary evaporator, silica gel column (ethyl acetate and petroleum ether, the volume ratio of 1: 3) to give the product 109mg, yield 68% , the following reaction formula:

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; Wenzhou Medical College; Xia, Qinqin; Fu, Lili; Bao, Xiaodong; Liu, Zhiguo; Liang, Guang; (11 pag.)CN105693621; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics