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. 626-43-7, name is 3,5-Dichloroaniline, This compound has unique chemical properties. The synthetic route is as follows., 626-43-7

Benzoyl acetone (0.165 g, 1.017 mmol) was dispersed over Montmorillonite K-10 catalyst (1.5 g) and a mixture of 3.5-dichloroaniline (0.552 g, 3.407 mmol) with 20 ml THF was added dropwise, while stirring. The reaction was stirred at room temperature for 48 h. The catalyst was removed by filtration and the solvent was removed on a rotary evaporator, yielding a dark red oil.Yield 93%. Colour: dark red. UV: lambdamax 359 nm, epsilonmax 29453 mol-1dm3cm-1 (CH3CN), 1H NMR (300 MHz, CDCl3, 25C):delta 7.91-7.89 ppm (d, aromatic, 2H); 7.54-7.44 ppm (m, aromatic,3H); 6.75-6.74 ppm (t, aromatic, 1H); 6.56 ppm (d, aromatic, 2H);6.20 ppm (s, CH, 1H); 2.22 ppm (s, CH3, 3H).

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; Ngake, Tankiso Lawrence; Potgieter, Johannes Hermanus; Conradie, Jeanet; Electrochimica Acta; vol. 296; (2019); p. 1070 – 1082;,
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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. 83121-15-7, name is 3,5-Dichloro-2,4-difluoroaniline, A new synthetic method of this compound is introduced below., 83121-15-7

To a mixture of 3,5-dichloro-2,4-difluoroaniline (5.0 g), an aqueous 57% solution of hydroiodic acid (20 ml) and water (20 ml), copper iodide (1.92 g) was added. The reaction liquid was maintained at 30C or less in a water bath.To the reaction mixture was added dropwise a water solution (2 mL) of sodium nitrite ( 1.74 g). The reaction mixture was stirred for 10 minutes, maintained at 30C or less in a water bath. To the reaction mixture was added dropwise a water solution (2 mL) of sodium nitrite (1.74 g), again. The reaction mixture was further stirred for 10 minutes, maintained at 30C or less in a water bath. To the reaction mixture was added dropwise a water solution (2 mL) of sodium nitrite (1.74 g), again. t-Butyl methyl ether was added and the mixture was washed with water and with an aqueous solution of sodium sulfite and brine, and dried over anhydrous magnesium sulfate. The drying agent was filtered off, the solvent was distilled off under reduced pressure and the residue was purified by silica gel chromatography (n- hexane) to obtain l,3-dichloro-2,4-difluoro-5-iodobenzene (6.0 g). i-NMR (CDC13) delta: 7.6-7.75 (1H, m).

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; BAYER CROPSCIENCE AG; MIHARA, Jun; HATAZAWA, Mamoru; YAMAZAKI, Daiei; KISHIKAWA, Hidetoshi; DOMON, Kei; WATANABE, Hidekazu; SASAKI, Norio; MURATA, Tetsuya; ARAKI, Koichi; SHIMOJO, Eiichi; ICHIHARA, Teruyuki; ISHIKAWA, Tadashi; SHIBUYA, Katsuhiko; GOeRGENS, Ulrich; BRUeCHNER, Peter; FISCHER, Reiner; JANSEN, Johannes-Rudolf; KAPFERER, Tobias; MAECHLING, Simon; MAUE, Michael; VOERSTE, Arnd; WO2012/35011; (2012); A1;,
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108-37-2, 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 108-37-2 as follows.

General procedure: Na2CO3 (212 mg, 2 mmol), 4-chloronitrobenzene (1 mmol) and styrene (1.5 mmol) were added successively into a dried Schlenk tube under nitrogen. Then the DMA (0.1mL) solution of DADPP (0.002mmol) and [Pd(C3H5)Cl]2 (0.0005mmol), which was reacted at 100C for 10 min prior to use, was added into the mixture. The reaction was performed at 130C. At the end of reaction, the mixture solution was extracted with ethyl acetate (3¡Á5 mL). Combined organic phase was washed with brine (3¡Á5mL) and dried over MgSO4. The dried solution was filtered and purified with silica gel chromatography (petroleum ether 60-90C) to give a corresponding product.

According to the analysis of related databases, 1-Bromo-3-chlorobenzene, the application of this compound in the production field has become more and more popular.

Reference:
Article; Jiang, Zhi-Jie; Wang, Wei; Zhou, Rong; Zhang, Lei; Fu, Hai-Yan; Zheng, Xue-Li; Chen, Hua; Li, Rui-Xiang; Catalysis Communications; vol. 57; (2013); p. 14 – 18;,
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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. 1193-72-2 name is 1-Bromo-2,4-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. 1193-72-2

Part C. tert-butyl (7bR,11aS)-6-(2,4-dichloroanilino)-1,2,7b,10,11,11a-hexahydro-4H-pyrido[4,3-b][1,4]thiazepino[6,5,4-hi]indole-9(8H)-carboxylate. An oven dried three-necked round bottom flask was fitted with septa, condenser, and a stopper. The flask was charged with tert-butyl (7bR,11aS)-6-amino-1,2,7b,10,11,11a-hexahydro-4H-pyrido[4,3-b][1,4]thiazepino[6,5,4-hi]indole-9(8H)-carboxylate (134 mg, 0.36 mmol), 1-bromo-2,4-dichlorobenzene (70 mg, 0.31 mmol), NaOtBu (60 mg, 0.62 mmol), and anhydrous toluene (5 mL). The solution was purged with argon at 80 C. for 25 min then cooled to room temperature. While maintaining a blanket of argon, Pd2(dba)3 (3.4 mg, 3.7 mumol), and BINAP (7 mg, 11.2 mumol) were added quickly. The resulting mixture was heated to 80 C. for 20 hours under argon while monitoring the consumption of starting material by TLC (50% ethyl acetate/hexanes). After cooling to room temperature, the dark solution was diluted with ethyl ether (10 mL) and filtered through a pad of silica, washing with ether and ethyl acetate. The resulting solution was concentrated and chromatographed (Combiflash, 95:5 to 75:25 hexanes/ethyl acetate gradient) yielding the title compound (78 mg, 48%) as a tan solid. 1H NMR (CDCl3, 300 MHz) delta 1.41 (s, 9H), 1.79-1.97 (m, 2H), 2.85-3.18 (m, 6H), 3.46-3.61 (m, 4H), 3.68 (s, 2H), 5.84 (s, 1H), 6.71 (d, 1H, J=1.9 Hz), 6.79 (d, 1H, J=1.8 Hz), 6.89 (d, 1H, J=8.8 Hz), 7.01 (dd, 1H, J=2.3, 8.8 Hz), 7.29 (d, 1H, J=2.3 Hz) ppm.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2,4-dichlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Robichaud, Albert J.; Fevig, John M.; Mitchell, Ian S.; Lee, Taekyu; Chen, Wenting; Cacciola, Joseph; US2004/186094; (2004); A1;,
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A common heterocyclic compound, 2770-11-8, name is 2-(4-Chlorophenoxy)aniline, molecular formula is C12H10ClNO, 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. 2770-11-8.

2-(4-Chlorophenoxy)aniline (200 mg, 0.9107 mmol, 1.1 eq) and JV-(3-acetylphenyl)-iV- ethylacetamide (169 mg, 0.827 mmol, 1 eq) were stirred in dry dichloromethane (DCM) at room temperature for 10 min. Tri-isopropoxytitanium chloride (395 muL, 1.654 mmol, 2 eq) was added to the reaction mixture which was stirred at room temperature for 16 hours. Sodium triacetoxyborohydride (700 mg, 3.308 mmol, 4 eq) was then added to the reaction mixture and was stirred at room temperature for a further 24 h. The reaction mixture was then poured onto a solution of saturated aqueous sodium bicarbonate (100 mL) and extracted with DCM (120 mL). The organic layer was washed with brine (120 mL), dried over MgSO4, filtered and concentrated to give the crude as a yellow oil. Purification of the crude by flash chromatography (ISCO) eluting with a gradient [from 25% ethyl acetate in petrol ether to 50% ethyl acetate in petrol ether] gave (87 mg, 26 %) as a white solid. 1H NMR (270 MHz, CDCl3) delta 1.05 (3H, t, J = 8.1 Hz, CH3), 1.49 (3eta, d, J = 6.4 Hz CH3), 1.67 (3H, s, CH3), 3.68 (2H, q, J= 8.1 Hz, CH2), 4.45-4.60 (2H, m, NH and CH) 6.37 (1eta, d, J = 8.2 Hz, ArH), 6.57 (IH, dt, J = 1.4, 8.2 Hz ArH), 6.75-7.06 (6H, m, ArH), 7.23-7.39 (4H, m, ArH); 13C NMR (67.5 MHz, CDCl3) delta 13.1, 22.8, 25.0, 43.8, 52.8, 112.0, 112.9, 117.2, 118.7, 119.3, 125.0, 126.1, 126.5, 128. 0, 129.8, 130.0, 138.0, 139.1, 142.8, 147.1, 156.5, 169.9 LCMS (90% MeOH and 10% H2O; Symmetry C18 reverse phase column) tr = 2.88 min; (ES+), m/z 409.2 (35ClM’, 75%), 383 (37ClM’, 25%); HRMS (ESI) calcd. for C24H25ClN2O2 (M+H)+ 409.1605, found 409.1689. 99.48% purity.

The synthetic route of 2-(4-Chlorophenoxy)aniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; STERIX LIMITED; WO2009/66072; (2009); A2;,
Chloride – Wikipedia,
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The chemical industry reduces the impact on the environment during synthesis 823-57-4, name is 2-Bromo-5-chloroaniline, I believe this compound will play a more active role in future production and life. 823-57-4

Step B: Preparation of l-Bromo-4-chloro-2-iodobenzene; [0828] A suspension of 2-bromo-5-chlorobenzenamine (1 1.348 g, 54.963 mmol) in concentrated HCl (100 mL) was cooled to 0C and treated dropwise over 20 minutes (using an addition funnel) with a solution of sodium nitrite (4.5506 g, 65.955 mmol) in water (20 mL). The reaction was stirred at 00C for 75 minutes. A solution of potassium iodide (27.372 g, 164.89 mmol) in water (50 mL) was added, and the reaction was stirred at 23C. After 1 hour, the reaction was heated to 700C. After 18 hours, the reaction was diluted with EtOAc (500 mL) and washed with water (300 mL), 2N NaOH solution (300 mL), saturated sodium thiosulfate solution (300 mL) and brine (250 mL), dried over MgSO4, concentrated in vacuo, and purified by silica gel chromatography (eluant: hexane) affording 1 1.1 1 g of 1 -bromo^-chloro^-iodobenzene.

The chemical industry reduces the impact on the environment during synthesis 823-57-4. I believe this compound will play a more active role in future production and life.

Reference:
Patent; AMGEN INC.; WO2008/76427; (2008); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 10061-02-6, name is trans-1,3-Dichloropropene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 10061-02-6

A suspension of 6.66 g (0.06 mol) of (E)-1,3-dichloropropene (3), 13.82 g (0.1 mol) of potassium carbonate, and 2.53 g (0.031 mol) of ethylamine hydrochloride in 75 mL of anhydrous acetonitrile was slowly heated to the boiling point with stirring and was then refluxed until complete conversion of 3 (12-14 h, GLC monitoring). The mixture was cooled and filtered, the precipitate was washed with ethyl acetate, the organic fractions were combined and concentrated, and the product was isolated by vacuum distillation. Yield 4.24 g (73%), bp 89 C (4-5 mm). IR spectrum, nu, cm-1: 2971, 2935,2811, 1635, 1456, 1360, 1285, 1132, 934, 801. 1H NMR spectrum, delta, ppm: 1.03 t (3H, CH3, J =7.2 Hz), 2.50 q (2H, CH3CH2N, J = 7.2 Hz), 3.09 d (4H, CH2CH=, J = 6.8 Hz), 5.93 d.t (2H, CH2CH=, Jtrans = 13.2, 6.8 Hz), 6.12 d (2H, ClCH=, Jtrans = 13.2 Hz). 13C NMR spectrum, deltaC, ppm: 11.94 (CH3), 46.80 (CH3CH2N), 52.74 (2C, CH2CH=), 119.99 (2C, ClCH=), 130.41 (2C, CH2CH=). Mass spectrum, m/z (Irel, %): 193 (5) [M]+, 180 (20), 178 (32), 132 (17), 77 (33), 75 (100), 68 (49), 56 (10), 49 (9), 42 (13), 39 (29).

The synthetic route of 10061-02-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shakhmaev; Sunagatullina, A. Sh.; Zorin; Russian Journal of Organic Chemistry; vol. 53; 6; (2017); p. 832 – 835; Zh. Org. Khim.; vol. 53; 6; (2017); p. 818 – 820,3;,
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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. 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 1996-30-1

Step 1. l-(2-Bromo-4-chlorophenyl)-lH-l,2,3-triazole. To a solution of 2-bromo-4-chloro-l- fluorobenzene (5 g, 24 mmol) and 2H-l,2,3-triazole (6.60 g, 95 mmol) in DMF (2 mL) was added K2CO3 (16.50 g, 119 mmol). The mixture was stirred at 100C for 13 h under N2 atmosphere. The mixture was diluted with water (10 mL) and extracted with EtOAc (10 mL x 2). The combined organic layers were dried over sodium sulfate and concentrated. The residue was purified by column chromatography (Si02, PE: EtOAc = 100: 1 to 3: 1) to give the title compound. MS (ESI) m/z 260.0 (M+H).

The synthetic route of 1996-30-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; LIU, Weiguo; EDMONDSON, Scott, D.; GUO, Zhuyan; MERTZ, Eric; OGAWA, Anthony, K.; SO, Sung-Sau; SUN, Wanying; BROCKUNIER, Linda, L.; ALI, Amjad; KUANG, Rongze; WU, Heping; WO2015/183709; (2015); A1;,
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The chemical industry reduces the impact on the environment during synthesis 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, I believe this compound will play a more active role in future production and life. 56961-77-4

Example 1 1- (2, 3-DICHLOROPHENYL)- [1, 4] diazepine (starting material) 2.25 g (10 MMOL) 1-bromo-2, 3-dichloro-benzene was dissolved in dry toluene (50 ml), 2.3 (11 MMOL) of [1, 4] diazepine-1-carboxylic acid tert-butylester was added followed by 0.2 g BINAP (2,2-bis (diphenylphosphino)-1, 1′-binaphtyl), 85 mg tris (DIBENZYLIDENEACETONE) dipalladium (0) and 1.2 g (12MMOL) SODIUM-TERT-BUTOXYDE. The reaction mixture was refluxed for eight hours and filtered. The organic layer was washed with water, dried and evaporated in vacuo. The residue was purified by chromatography and deprotected at 10 C using 20 ML ETHYLACETATE saturated with gaseous hydrochloric acid, the precipitate was filtered giving 2.1 g (yield : 75 %) hydrochloride salt of the title compound, melting at 182-3 C.

The chemical industry reduces the impact on the environment during synthesis 56961-77-4. I believe this compound will play a more active role in future production and life.

Reference:
Patent; RICHTER GEDEON VEGYESZETI GYAR RT.; WO2005/12266; (2005); A1;,
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A common heterocyclic compound, 108-41-8, name is 1-Chloro-3-methylbenzene, molecular formula is C7H7Cl, 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. 108-41-8.

General procedure: The typical procedure is as follows. Oven dried Schlenk tube was equipped with stirrer bar, was charged with aryl halides (1 mmol), acrylates (1.2 mmol), K2CO3 (2 mmol) and catalyst2 (3 mol %) in DMF medium. The reaction mixture was stirred in an oil bath at 100C under argon atmosphere for an appropriate period of time. After completion of the reaction, the reaction mixture was then cooled to room temperature and diluted with Et2O/H2O(1:1, 20 mL). The organic layer was alienated and dried with anhydrous MgSO4. The product was filtered and dried under vacuum. The resulting crude compound was purified by column chromatography on silica gel to afford the corresponding products.

The synthetic route of 1-Chloro-3-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Nirmala, Muthukumaran; Arruri, Sathyanarayana; Vaddamanu, Moulali; Karupnaswamy, Ramesh; Mannarsamy, Maruthupandi; Adinarayana, Mannem; Ganesan, Prabusankar; Polyhedron; vol. 158; (2019); p. 125 – 134;,
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