Author: Jessica.F

Synthetic Route of 112-26-5, A common heterocyclic compound, 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane, molecular formula is C6H12Cl2O2, 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.

A mixture of 3.2 g (10.1 mmol) of sodium 2-(diphenylphosphoryl) phenolate [10] and 0.93 g (5.0 mmol) of 1,8-dichloro-3,6-dioxaoctane in 7 mL of anhydrous dioxane was placed into the laboratory system with focused microwave heating in hermetically closed glass vial. The mixture was heated at 150C (50 W) for 0.6 h. After cooling, the reaction mixture was poured into 50 mL of water, acidified with conc. HCl to pH 1, and extracted with CHCl3 (3 ¡Á 30 mL). The extract was washed with dilute HCl (2 ¡Á 30 mL), and water (3 ¡Á 35 mL), and evaporated ina vacuum. To the residue 20 mL of diethyl ether was added, and the precipitate was filtered off. The filtrate was chromatographed.

The synthetic route of 112-26-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Baulin; Ivanova; Polyakova; Pyatova; Krivorot’ko; Tsivadze; Russian Journal of General Chemistry; vol. 85; 4; (2015); p. 899 – 905; Zh. Obshch. Khim.; vol. 85; 4; (2015); p. 899 – 905,7;,
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Electric Literature of 13078-79-0, 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. 13078-79-0, name is 2-(3-Chlorophenyl)ethanamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Under nitrogen atmosphere, ethanol (30 mL), immediate III (3 mmol) and titanium (IV) isopropoxide (9 mmol) were added to a three-necked round bottom flask and stirred for 0.5 h, then the substituted ethylamine (3 mmol) was dropped into the solution and stirred for 3 h at room temperature. Subsequently, sodium borohydride (4.5 mmol) was added to the flask slowly, the reductive amination reaction was maintained for 3 h. According to the TLC monitoring results, the ammonia water (2 mol L-1, 10 mL) was poured into the flask to quench the reaction. The resulting mixture was filtered in vacuum and evaporated on rota vapor (Buchi). Hereafter, dissolved the residue with ethyl acetate (50 mL), and the solution was washed with 2 mol L-1 hydrochloric acid (30 mL), saturated aq NaHCO3 solution (30 mL), and brine (40 mL), successively, dried over anhydrous Na2SO4 and filtered. Solvent was evaporated in vacuum, and the residue was purified by silica gel column chromatography (petroleum ether / ethyl acetate as eluents). Finally, the samples were recrystallized from ethyl acetate / petroleum ether to afford target compounds with higher purity.

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-(3-Chlorophenyl)ethanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Cai, Nan; He, Lu; Wang, Kai; Feng, Zhihui; Cui, Zining; Ji, Mingshan; Qi, Zhiqiu; Qin, Peiwen; Li, Xinghai; Bioorganic and Medicinal Chemistry Letters; vol. 30; 4; (2020);,
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Synthetic Route of 461432-23-5, 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. 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 1.6 M n-BuLi in hexanes (0.1 mL, 0.158 mmol) was added dropwise at -78 C to a stirred solution of compound 15 (50 mg, 0.158 mmol) in dry THF (2.5 mL) and the mixture was stirred at this temperature for 45 min. Then, a solution of amide 22 (100 mg, 0.158 mmol, 1 eqiv.) in THF (1 mL) was added dropwise to this mixture at the same temperature, the resulting mixture was stirred at this temperature for another 1 h, and then left at ambient temperature for 2 days. Then, the mixture was cooled in an ice bath, a saturated aqueous solution of NH4Cl (3 mL) was added and the mixture was extracted with DCM (3 * 5 mL). The combined organic layers were dried over Na2SO4, the solvent was removed under reduced pressure and the residue was chromatographed on a silica gel column (hexane/ethyl acetate 10:1) to give product 2 (45 mg, 35%) as a colorless oil.

The synthetic route of 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Triantakonstanti, Virginia V.; Mountanea, Olga G.; Papoulidou, Kyriaki-Eleni C.; Andreou, Thanos; Koftis, Theocharis V.; Gallos, John K.; Tetrahedron; vol. 74; 39; (2018); p. 5700 – 5708;,
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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. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 60811-21-4

Add 2-chloro-1-fluoro-4-bromobenzene (0.10 mol) to a 250 mL round bottom flask and dissolve in DMF (100 mL). Add potassium carbonate (0.20 mol) and di-n-hexylamine (0.10 mol) with stirring. The reaction system was heated to 90 C for 72 hours. After completion of the reaction, the mixture was cooled to room temperature, filtered, and the organic phase was concentrated to 50 mL, poured into dichloromethane (150 mL), washed with water (150 mL¡Á3) and brine (150 mL) The sodium was dried, and the solvent was evaporated under reduced pressure. and the crude material was purified by column chromatography to yield N, N-dihexyl-2-chloro-4-bromoaniline.

The synthetic route of 60811-21-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ocean University of China; Shao Changlun; (69 pag.)CN108658937; (2018); A;,
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Application of 56961-77-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 56961-77-4 name is 1-Bromo-2,3-dichlorobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To 1-bromo-2,3-dichlorobenzene [r-1] (22.6 g, 100 mmol), sodium t-butoxide (29.6 g, 308 mmol), 2,2?-bis (diphenylphosphino)-1 , 1 ?-binaphthyl [I3INAP] (2.51 g, 4.0 mmol), bis(dibenzylideneacetone) palladium (0) [Pd2 (dba) 31(1.83 g, 2.0 mmol), and toluene (400 ml), aniline [r-2] (18.5 ml, 203 mmol) was added under a nitrogen atmosphere at room temperature, and the resulting mixture was heated and stirred at 1000 C. for 26 hours. The reaction solution was cooled to room temperature, and was filtered using silica gel column chromatography, and a solvent was distilled oil under reduced pressure to obtain a crude product. Thereafier, the resulting crude product was washed with toluene to obtain 2-chloro-N,N?-diphenyl- 1 ,3-benzenediamine [r-3] (18.4 g, yield 63%) as a white solid. The structure of the compound thus obtained was identified with an NMR spectrum. 1H-NMR (400 MHz, CDC13): &6.08 (s, 2H), 6.80 (s, 2H), 6.99 (t, 1H), 7.04 (U, J=1.1, 7.3 Hz, 2H, (CH)2CH (CR2)2), 7.18 (dd, 4H), 7.32 (dd, 4H). 13C-NMR (101 MHz, CDC13): 107.1 (2C), 109.4,120.4 (4C), 122.5 (2C), 127.0, 129.3 (4C), 141.1 (2C), 141.6 (2C).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2,3-dichlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Kwansei Gakuin Educational Foundation; JNC Corporation; Hatakeyama, Takuji; NAKATSUKA, Soichiro; GOTOH, Hajime; SASADA, Yasuyuki; YANAI, Motoki; IKUTA, Toshiaki; (337 pag.)US2018/69182; (2018); A1;,
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Adding a certain compound to certain chemical reactions, such as: 139512-70-2, name is 4-Chloro-5-fluorobenzene-1,2-diamine, 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 139512-70-2, category: chlorides-buliding-blocks

General procedure: A mixture of compounds 1a-l (0.013 mol) and 4-chloro-5-fluoro-ophenylenediamine(2) (0.01 mol) in methanol (10 mL) was irradiatedwith ultrasonic irradiation at 50 C for 7 min (8 min for 3a) Afterreaction completion (monitored by TLC, ethyl acetate/hexane = 3:1), themixture was poured onto water and the precipitated product was filtrated off, washed with water and recrystallised from ethanol/water, 3:1.

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:
Article; Mente?e, Emre; Kahveci, Bahittin; Mente?e, Meltem; Journal of Chemical Research; vol. 42; 6; (2018); p. 329 – 331;,
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Adding a certain compound to certain chemical reactions, such as: 2613-34-5, name is 3-Chloro-2,4-difluoroaniline, 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 2613-34-5, name: 3-Chloro-2,4-difluoroaniline

A mixture of 2,4-dichloropyrimidine (6.0 g, 40.5 mmol), 3-chloro-2,4-difluoroaniline (6.28 g, 38.5 mmol), diisopropylethylamine (9.16 ml, 52.7 mmol) and pentanol (20 ml) was refluxed for 24 hrs. After concentration under reduced pressure, the residue was dissolved in ethyl acetate and the solution washed with water, dried and concentrated. The crude material was triturated in methylene chloride and the white solid collected by filtration to give 2.1 g of the desired product. The filtrate was concentrated and purified on silica gel (10 to 50% EtOAc in petroleum ether) to give another 1.9 g of material (total yield 4.0 g, 36%). NMR Spectrum (500 MHz, DMSOd6) 6.80 (d, IH), 7.38 (ddd, IH), 7.74 (ddd, IH), 8.21 (d, IH), 9.95 (bs, IH); Mass Spectrum MH+ 276.

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, 3-Chloro-2,4-difluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2008/104754; (2008); A1;,
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Application of 19752-55-7, 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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Add 2.2 g of 1-bromo-3,5-dichlorobenzene (0.01 mol) to the reaction flask. 2.3 g of potassium 2,2,2-trifluoroacetate (0.015 mmol), 2.3 g of iodinated ketone (0.012),1.04 g of pyridine (0.013 mol), 10 ml of N-methylpyrrolidone, refluxed at 200 C for 1 hour, and the solvent was evaporated to give a crude compound 1.94 g. Then, after mixing 10 ml of H2SO4 and 5 ml of HNO3, the crude compound 1 was slowly added at 0 C. After the reaction for 2 hours, the reaction was stopped, and the mixture was poured into ice water and suction filtered to give the desired fipronil intermediate 2.19 g in a yield of 86.2%.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-3,5-dichlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Jiangsu Changqing Agrochemical Co., Ltd.; Yu Guoquan; Sun Xialin; Ma Changqing; Ding Huaping; (5 pag.)CN109369403; (2019); A;,
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Adding a certain compound to certain chemical reactions, such as: 928783-85-1, name is 1-Bromo-3-chloro-5-(trifluoromethyl)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 928783-85-1, Formula: C7H3BrClF3

A solution of 1-bromo-3-chloro-5-(trifluoromethyl)benzene (5.0 g), 3-hydroxypyrrolidine (1.85 g), palladium(II) acetate (217 mg), (+/-)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (1.2 g) and cesium carbonate (18.8 g) in toluene (96 mL) was stirred under an argon gas atmosphere at 85 C. for 16 hr. After cooling to room temperature, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate 80:20-10:90) to give the title compound (4.11 g, yield 80%) as a brown oil.1H-NMR (300 MHz, CDCl3) delta: 1.65 (d, J=3.8 Hz, 1H), 2.00-2.29 (m, 2 H), 3.19-3.32 (m, 1H), 3.38 (td, J=8.7, 3.4 Hz, 1H), 3.45-3.60 (m, 2H), 4.58-4.72 (m, 1H), 6.61 (s, 1H), 6.63-6.68 (m, 1H), 6.88 (s, 1H).

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-Bromo-3-chloro-5-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Kasai, Shizuo; Kamaura, Masahiro; Cho, Nobuo; US2011/251187; (2011); A1;,
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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. 27139-97-5, name is 2-Bromo-4-chloro-1-methylbenzene, A new synthetic method of this compound is introduced below., Safety of 2-Bromo-4-chloro-1-methylbenzene

Step 1 5-chloro-2-methylbenzaldehyde To a solution of 2-bromo-4-chlorotoluene (20.0 g; 97.3 mmol) in 300 mL of THF at -78¡ã C. was added dropwise a 2.5 M solution of n-BuLi (102.2 mmol). After 30 min of stirring at that temperature, 1-formylpiperidine (11.4 mL) in 10 mL of THF was added and the solution left for 1 h. It was brought to 0¡ã C., quenched with NH4OAc (25percent) and diluted with EtOAc. The organic phase was dried over Na2SO4, filtered and the solvent removed to yield 13.3 g of the title compound. 1H NMR (CDCl3) delta2.6 (3H, s), 7.15 (1H, d), 7.4 (1H, d), 7.75 (1H, s) and 10.2 (1H, s).

The synthetic route of 27139-97-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck Frosst Canada & Co.; US6242493; (2001); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics