Tag: M.W=100-200

Reference of 1435-48-9, A common heterocyclic compound, 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene, molecular formula is C6H3Cl2F, 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.

Step 1. 1-(2,4-Dichlorophenyl)piperazine A mixture of 1,3-dichloro-4-fluorobenzene (Aldrich; 4.21 g), piperazine (Aldrich; 11.0 g), and N,N-dimethylacetamide (Aldrich; 15 mL) is heated at 165 C. for 6.5 h. After cooling, the mixture is partitioned between dichloromethane and aq. sodium bicarbonate. The organic layers are dried over sodium sulfate and concentrated under reduced pressure to give 4.48 g of 1-(2,4-dichlorophenyl) piperazine. 1 H NMR (CDCl3) delta3.00, 3.06, 6.96, 7.19, 7.36.

The synthetic route of 1435-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pharmacia & Upjohn Company; US5912246; (1999); A;,
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Adding a certain compound to certain chemical reactions, such as: 622-24-2, name is (2-Chloroethyl)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 622-24-2, Product Details of 622-24-2

General procedure: General Procedure: In a 10 mL Schlenk tube were placed CoBr2 (0.3 M in THF, 0.10 mL, 0.030mmol), 1,3-diisopropylbenzimidazolium bromide (L2, 8.5 mg, 0.030 mmol), 2-alkenylpyridine(0.30 mmol), alkyl chloride (0.45 mmol), N,N,N,?N?-tetramethylethylenediamine (90 muL, 0.60mmol) and THF (0.28 mL). To the mixture was added a THF solution of tBuCH2MgBr (0.96 M,0.63 mL, 0.60 mmol) dropwise at 0 C. The resulting mixture was stirred at room temperature for12 h, and then quenched by the addition water (1.0 mL). The organic layer was separated, and the aqueous layer was extracted with ethyl acetate (3 x 3 mL). The combined organic layer was dried over Na2SO4 and concentrated under reduced pressure. The crude product was purified by silicagel chromatography to afford the alkylation product.

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Reference:
Article; Yamakawa, Takeshi; Seto, Yuan Wah; Yoshikai, Naohiko; Synlett; vol. 26; 3; (2015); p. 340 – 344;,
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Related Products of 108-70-3, A common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, molecular formula is C6H3Cl3, 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 1 L three-necked flask is charged with 100 g (551 mmoles) of 1,3,5-trichlorobenzene that is placed in suspension in 400 mL of dimethylsulfoxide. This suspension is heated to 80 C., under agitation, then 119.06 g of a 30% solution of sodium methanolate are added drop-wise, i.e. 661.2 mmoles of sodium methanolate. Heating is continued up to 90 C., still under agitation, for 3 hours 10. After this time, the content of the flask is lowered too ambient temperature and it is poured into 4 L of iced water. A white solid is precipitated. This solid is recovered by filtering, washed three times with 250 mL of iced water, then vacuum died at ambient temperature. This gives 95.55 g of 3,5-dichloroanisole in the form of a white powder whose analysis by GC-MS (under the same conditions as previously) shows that it has a degree of purity of 96%. The yield is 98%.

The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Commissariat a l’energie atomique et aux energies alternatives; Pasquinet, Eric; Wuillaume, Anne; Poullain, Didier; Kosciusko-Morizet, Etienne; US2013/178655; (2013); A1;,
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Reference of 51114-68-2,Some common heterocyclic compound, 51114-68-2, name is 3-Chloro-2-methoxyaniline, molecular formula is C7H8ClNO, 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 four-necked flask was added 30 g (0.19 mol) of 3-chloroanisidine,30 g (1.67 mol) of water was added and the temperature was raised to 50 C,A solution of 36% HC1231 g (2.28 mol)After incubation for 0.5 h,The temperature was lowered to 0 C, and 30% NaN0244 was slowly added dropwise.Diazotization reaction,Upon completion of the addition,After 2h incubation,Remove the filter cake. 69.5 g (0.38 mol) of 48% HBF4 solution was added dropwise to the filtrate,To carry out condensation reaction,Insulation lh later.The solution was filtered,The solids were dried for dehydration.The dried fluoroborate,Slowly heated to 130 C for cracking reaction,Until no gas is produced.After the cracking of the solution for distillation,The 2,6-CFA fraction was collected to give 26 g of the title compound. Purity> 98.5%,The yield of 3 steps was 85% (from 2,3-dichloronitrobenzene to the final target compound,The overall yield was 69.4%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Chloro-2-methoxyaniline, its application will become more common.

Reference:
Patent; JIANG SU LIANHE CHEMICAL TECHNOLOGY CO LTD; LIANHE CHEMICAL TECHNOLOGY (YANCHENG )CO LTD; LIANHE CHEMICAL TECHNOLOGY (SHANGHAI )CO LTD; FAN, XIAOBIN; ZHANG, JUNTAO; XU, XIAOMING; WANG, HUI; YANG, JUN; SHEN, QIFU; (10 pag.)CN103787846; (2016); B;,
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Synthetic Route of 36556-52-2, These common heterocyclic compound, 36556-52-2, name is 2,3-Dichloro-4-fluoroaniline, 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 vial containing 2,3-dichloro-4-fluoroaniline (307.4 mg, 1.7 mmol) in 2 mL toluene was added 4M HCl in 1,4-dioxane (0.43 mL, 1.7 mmol) followed by phosgene (20% in toluene; 3.6 mL, 6.8 mmol). Precipitate formed upon HCl addition. The vial was capped and heated to 100 C. After 30 min, all the solids had disappeared. After 6.5 h, the solvent was removed under vacuum. Material was re-dissolved in toluene, and solvent was again removed under vacuum to eliminate any remaining phosgene. The resulting material was a brown oil that crystallized upon standing and was used without further purification. A capped vial containing 7 (108.8 mg, 0.55 mmol) and 2,3-dichloro-1-fluoro-4-isocyanatobenzene from above (~0.55 mmol) was heated to 70 C. After 2 days, solvent was removed under vacuum. The oil residue was treated with DCM, producing a precipitate. The resulting mixture was left to stand at room temperature for >30 min. The solids were filtered, washed with minimal amount of DCM and dried under vacuum to give119.1 mg (54%) of 8k as an off-white solid. The material was used without further purification.

The synthetic route of 36556-52-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Moffett, Kristofer; Konteatis, Zenon; Nguyen, Duyan; Shetty, Rupa; Ludington, Jennifer; Fujimoto, Ted; Lee, Kyoung-Jin; Chai, Xiaomei; Namboodiri, Haridasan; Karpusas, Michael; Dorsey, Bruce; Guarnieri, Frank; Bukhtiyarova, Marina; Springman, Eric; Michelotti, Enrique; Bioorganic and Medicinal Chemistry Letters; vol. 21; 23; (2011); p. 7155 – 7165;,
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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. 2106-04-9, name is 3-Chloro-2-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3-Chloro-2-fluoroaniline

[00178] Synthesis of isothiocyanate 3c[00179] Preparation of compound 18[00180] A solution of compound 17 (5g, 0.034mol) in DMF (50mL) was added a DMF solution (50mL) of NBS (6.05 g, 0.034 mol) drop-wise at room temperature. After 16h, the reaction mixture was diluted with ethyl acetate (lOOmL) and washed with brine (2xl00mL). The separated organic phase was dried over Na2S04 and concentrated to give the title compound 18 as an oil (5.0g, 65% yield). ESI-MS (M+H)+: 223.92.

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 2106-04-9.

Reference:
Patent; SUZHOU KINTOR PHARMACEUTICALS,INC.; TONG, Youzhi; WO2012/119559; (2012); A1;,
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Adding a certain compound to certain chemical reactions, such as: 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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 4584-46-7, Recommanded Product: 4584-46-7

A mixture of 2-(2,4-dimethoxy-benzyl)-4-hydroxy-isoindole-1,3-dione (317 mg, 1.01 mmol), 2- dimethylaminoethyl chloride hydrochloride (160 mg, 1.11 mmol) and potassium carbonate (350 mg, 2.5 mmol) in DMF (4 ml_) was heated at 6O0C for 18 hours. The mixture was concentrated in vacuo, taken up in ethyl acetate and extracted twice with 1 N hydrochloric acid. The aqueous extracts were made basic with solid potassium carbonate and extracted with ethyl acetate (*2). The combined organic extracts were washed with brine, dried (MgSO4) and concentrated to give the title compound (236 mg, 61 %) as an off-white solid. 1H NMR (methanol-d4) 7.73 (1 H, t), 7.44-7.40 (2H1 m), 7.02 (1 H, d), 6.51 (1 H, d), 6.42 (1 H, dd), 4.72 (2H, s), 4.33 (2H, t), 3.80 (3H, s), 3.76 (3H, s), 2.87 (2H, t), 2.40 (6H, s). MS: [M+H]+ 385.

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; ASTEX THERAPEUTICS LIMITED; WO2008/44054; (2008); A2;,
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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. 106-39-8, name is 1-Bromo-4-chlorobenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Bromo-4-chlorobenzene

A flame-dried Schlenk flask was charged with tris(dibenzylideneacetone)palladium (4.6 mg, 0.005 mmol), 1 (4.4 mg, 0.025 mmol) or 6a (11.9 mg, 0.025 mmol), sodium terf-butoxide (134 mg, 1.40 mmol) and toluene (2.0 ml_) under nitrogen. Aryl bromide (1.00 mmol) and amine (1.10 mmol) were added and the resulting red solution heated at 800C with rapid stirring until reaction was complete, as judged by GC analysis. The reaction mixture was allowed to cool to room temperature, diluted with diethyl ether, passed through celite and the solvent removed to leave a yellow solid. Known products were characterised by NMR spectroscopy and mass spectrometry and unknown products by NMR spectroscopy, mass spectrometry and high resolution mass spectrometry (HRMS). The conversions were calculated using GC analysis as an average over three repeats.

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; UNIVERSITY OF NEWCASTLE UPON TYNE; WO2009/138708; (2009); A1;,
Chloride – Wikipedia,
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Related Products of 918538-05-3,Some common heterocyclic compound, 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine, molecular formula is C6H3Cl2N3, 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 100 mL flask was added 2,4-dichloropyrrolo[2,1-f][1,2,4]triazine 23 (15.96 mmol), and tetrahydrofuran (40 mL). To the resulting solution was added sodium phenolate (17.55 mmol) portion wise. After 1 h, an aliquot of the reaction mixture was diluted with methanol and analyzed by LCMS to ensure complete conversion. The reaction mixture was concentrated. The residue was stirred with water, filtered, washed extensively with water and dried to obtain 2-chloro-4-phenoxypyrrolo[2,1-f][1,2,4]triazine 24.

The synthetic route of 918538-05-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Harikrishnan, Lalgudi S.; Warrier, Jayakumar; Tebben, Andrew J.; Tonukunuru, Gopikishan; Madduri, Sudhakara R.; Baligar, Vishweshwaraiah; Mannoori, Raju; Seshadri, Balaji; Rahaman, Hasibur; Arunachalam; Dikundwar, Amol G.; Fink, Brian E.; Fargnoli, Joseph; Fereshteh, Mark; Fan, Yi; Lippy, Jonathan; Ho, Ching-Ping; Wautlet, Barri; Sheriff, Steven; Ruzanov, Max; Borzilleri, Robert M.; Bioorganic and Medicinal Chemistry; vol. 26; 5; (2018); p. 1026 – 1034;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 95-51-2, These common heterocyclic compound, 95-51-2, name is 2-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.

A solution of 254 mg (2 mmol) of o-chloroaniline and 143 mg (1.2 mmol) of potassium bromide was added to a 50 ml three-necked flask, Into the AcOH: H2O = 9: 1 10ml solvent, transferred to the constant temperature magnetic stirring water bath, control the temperature of 30 stirring reactionOne hour, 1.8 g (1.8 mmol) of ZnAl-BrO3-LDHs was added slowly in portions 15 minutes before the reaction. After the reaction, use two The reaction mixture was extracted with methyl chloride and the organic phases were combined. Two syrups of silica gel (200-300 mesh) were added to the dichloromethane phase and Dichloromethane was distilled off under reduced pressure and separated by column chromatography (petroleum ether: ethyl acetate = 10: 1 as eluent) To pure product 321 mg. The material was a gray solid with a yield of 78%

Statistics shows that 2-Chloroaniline is playing an increasingly important role. we look forward to future research findings about 95-51-2.

Reference:
Patent; Zhejiang University of Technology; Wang Ligeng; Chen Luqu; Zhang Hualong; Yu Qin; (11 pag.)CN107089919; (2017); A;,
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