Tag: M.W=100-200

Synthetic Route of 1005-56-7, These common heterocyclic compound, 1005-56-7, name is O-Phenyl carbonochloridothioate, 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: Phenyl chlorothionoformate (345 mg, 2.0 mmol), amine 2 (4.0 mmol) and water (15 mL) were added successively to a 50 mL round-bottom flask. The reaction mixture was stirred at room temperature for 1 h (monitored by TLC). After the reaction was complete, the solid was filtered off, washed with 10% HCl (2 ¡Á 20 mL) and deionised water(2 ¡Á 20 mL), and dried under vacuum to give the pure thiocarbamates 3. All products are known compounds and were identified by comparison of their physical and spectral data with those reported inthe literature.28

The synthetic route of 1005-56-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Zhengyi; Chen, Yuan; Yin, Yue; Wang, Zhiming; Sun, Xiaoqiang; Journal of Chemical Research; vol. 40; 11; (2016); p. 670 – 673;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 18655-50-0, 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 18655-50-0 as follows.

EXAMPLE 5 2-[N-(3-(p-Chlorophenyl)propylamino)]-5-hydroxy-4-methylpyrimidine [Formula I: R=H; R’=pCl-C6 H4 (CH2)3 ] A mixture of 2.5 g (0.02 mole) of 5-acetyl-2-aminooxazole, 10.5 g (0.062 mole) of 3-(p-chlorophenyl)propylamine, and 2.7 ml of water was heated at 110 C. (external) for 16 hours. The mixture was allowed to cool to room temperature and diluted with 15 ml of water. The resulting precipitate, which is 2-[N-(3-(p-chlorophenyl)propylamino)]-5-acetyl-1H-imidazole, was collected and set aside. Concentration of the filtrate afforded as oil which was chromatographed over silica gel using 1:1 ethyl acetate/hexane as eluent. The less polar material was the desired product which was isolated as a solid. Recrystallization from acetonitrile afforded 0.71 g (13%) of the title compound, mp 99-100 C.

According to the analysis of related databases, 18655-50-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pfizer Inc.; US4554276; (1985); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

39191-07-6, name is 1-(3-Chlorophenyl)-N-methylmethanamine, 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. COA of Formula: C8H10ClN

General procedure: To a solution of 1,4-bis(bromomethyl)benzene (1 mmol) in anhydrous acetonitrile (10 mL) was added potassium carbonate (3 mmol) and the corresponding secondary amine (2.2 mmol). The reaction mixture was heated at reflux for 3 h. The resulting mixture was diluted with water (20 mL) and extracted with ethyl acetate (15 mL) three times. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The crude was purified by column chromatography with methanol/dichloromethane (150:1, v/v) to give the title compound as a colorless liquid or a white solid.

The synthetic route of 39191-07-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bai, Renren; Liang, Zhongxing; Yoon, Younghyoun; Liu, Shuangping; Gaines, Theresa; Oum, Yoonhyeun; Shi, Qi; Mooring, Suazette Reid; Shim, Hyunsuk; European Journal of Medicinal Chemistry; vol. 118; (2016); p. 340 – 350;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 43141-66-8, name is 1-Chloro-4-(difluoromethyl)benzene, 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 43141-66-8, name: 1-Chloro-4-(difluoromethyl)benzene

Synthesis of compound 21 Bromine (17 muL; 0.34 mmol; 1.1 eq.) is added to a quartz reactor under an inert atmosphere, which is surmounted by a mercury vapour UV lamp equipped with a cooling system, and which contains a solution of para-chloro (difluoromethyl) benzene20 (50 mg; 0.3 mmol; 1 eq.) in carbon tetrachloride (5 mL; distilled over P2O5) and potassium carbonate (0.212 g; 1.54 mmol; 5 eq.). The reaction medium is refluxed and is irradiated for 5 h (84% conversion rate determined by GC). The mixture is then filtered and concentrated. The product 2j_ is involved in the following step without purification.2h C7H4BrClF2 M = 241.46 g.mol”1NMR 19F (CDO1. 282.5 Mz): – 43.9 (s, 2F). Mass: (IE): (M +) 240-242-244.

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; TFCHEM; WO2009/121939; (2009); A2;,
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