Month: February 2021

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 29671-92-9 as follows. Quality Control of Carbamimidic chloride hydrochloride

A mixture of anthranilic acid (8.9 g, 41.2 mmol), chloroformamidine hydrochloride (9.48 g), sulfolane (1.65 mL) and dimethylsulfone (19.8 g) was heated at 165C for 1 hour. Then, water was added (300 ml) to the hot reaction mixture and the pH was adjusted to 7-8 by the addition of a aqueous ammonia solution in water (25%). The precipitate was collected by filtration and resuspended in MeOH (100 mL). Filtration and drying of he obtained solid in the presence of P2O5, yielded 9.9 g (41.2 mmol, quant.) of the title compound as a solid. The crude product was used without further purification in the next step.

According to the analysis of related databases, 29671-92-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Smits, Rogier A.; Lim, Herman D.; Van Der Meer, Tiffany; Kuhne, Sebastiaan; Bessembinder, Karin; Zuiderveld, Obbe P.; Wijtmans, Maikel; De Esch, Iwan J.P.; Leurs, Rob; Bioorganic and Medicinal Chemistry Letters; vol. 22; 1; (2012); p. 461 – 467;,
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Adding a certain compound to certain chemical reactions, such as: 97329-43-6, name is 1-Bromo-2-chloro-3-methylbenzene, 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 97329-43-6, Formula: C7H6BrCl

General procedure: A mixture of arylaldehyde (0.1 g, 1 mmol), dihaloarene (0.565 g, 2 mmol), Pd(OAc)2 (0.022 g, 10.0 mol%), N-phenylpicolinamide (L7, 0.019 g, 15.0 mol%) and potassium hydrogen carbonate (0.5 g, 5 mmol) in tert-amyl alcohol (5.0 ml) was taken in 100.0 ml round bottom flask under N2 atmosphere and stirred for 120C for 24 h. Progress of the reaction was monitored continuously by TLC with ethyl acetate: hexane (2:3) eluent system. After completion of reaction, crude was poured into crushed ice and then filter the reaction mixture. Filtrate then extracted with ethyl acetate (3 times). Organic layer was separated, dried (over anhydrous Na2SO4) and evaporated under reduced pressure and purified by column chromatography to obtain desired product. Characterization data of compounds 3a, 3b, 3c, 3d, 3e, 3f, 3g, 3h, 3i, 3j, 3k, 3l, 3v and 3x were found exactly similar as reported in the literature (References of above compound are mentioned in Supplementary data).

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; Patel, Anuj; Shaikh, Mahommedumar; Chikhalia, Kishor; Tetrahedron; vol. 75; 2; (2019); p. 236 – 245;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 104-77-8, A common heterocyclic compound, 104-77-8, name is 3-Chloro-N,N-diethylpropan-1-amine, molecular formula is C7H16ClN, 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.

Example 29 (346) Synthesis of N-(Toluene4-sulfonyl)-L-prolyl-4-[3-(N,N-diethylamino)propoxy]-L-phenylalanine Methyl Ester The methyl ester was prepared via O-alkylation of N-(toluene-4-sulfonyl)-L-prolyl-L-tyrosine methyl ester with 3-diethylaminopropyl chloride in refluxing 2-butanone in the presence of potassium carbonate and sodium iodide. NMR data was as follows: 1H NMR (DMSO-d6, 400 Mhz): delta=1.0 (6H, bs); 1.4-1.6 (4H, m); 1.85 (2H, m); 2.18 (3H, s); 2.5 (2H, bs); 2.5-2.8 (4H, bs); 2.9 (2H, m); 3.1 (1H, dd, J=8, 10, 8 Hz); 3.35 (1H, dd, J=8, 4, 8 Hz); 3.6 (3H, s); 3.94 (2H, t, J=6, 6 Hz); 4.1 (1H, m); 4.48 (1H, dd, J=8, 6, 8 Hz); 6.8 (2H, d, J=10 Hz); 7.1 (2H, d, J=10 Hz); 7.4 (2H, d, J=10 Hz); 7.7 (2H, d, J=10 Hz); 8.2 (1H, d, J=10 Hz). MS: +ESI, m/z 560.5 ([MH]+, 100%).

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; Athena Neurosciences, Inc.; American Home Products Corp.; US6492421; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 626-43-7, name is 3,5-Dichloroaniline, molecular formula is C6H5Cl2N, 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. Quality Control of 3,5-Dichloroaniline

General procedure: In a 100 ml three-necked flask equipped with a thermometer and an electromagnetic stir bar were added 0.01 mol of anhydrous K2CO3 powder, 0.01 mol of 2-nitroaniline,30 ml of acetone,A solution prepared by dissolving 0.01 mol of 1,3-dimethyl-4-pyrazolecarboxylic acid chloride in 20 ml of acetone was gradually added dropwise at low temperature (0 to 5 C), and the reaction was continued at room temperature for 10 hours. The reaction mixture was filtered under reduced pressure, and the resulting filtrate was decompressed to yield a crude product of compound Q110907. The crude product of compound Q110907 was recrystallized from acetonitrile to give the compound (Q110907) in a yield of 42.9%. Using 3,5-dichloroaniline instead of 2-nitroaniline; Chloroform as the reaction solvent; the reaction temperature was 55 ¡À 5 C; reaction time was 5 hours, chlorobenzene recrystallization

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 626-43-7, its application will become more common.

Reference:
Patent; Qingdao Agricultural University; sun, Jia Long; (11 pag.)CN103524417; (2016); B;,
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Some common heterocyclic compound, 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, molecular formula is C6H3ClF2O2S, 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. COA of Formula: C6H3ClF2O2S

at room temperature,2-methyl-4-carbonyl-6,7,8,9-tetrahydropyrido [1,2-a] thiophene [2,3-d] pyrimidin-3-amine hydrochloride Compound 10 (0.31 g, 1m mol) was dissolved in anhydrous dichloromethane (10 ml), followed by addition3,5-difluorobenzenesulfonyl chloride (0.23 g, 1.1 mmol)Triethylamine (0.12 g, 1.2 mmol) was slowly added with stirring, stirred at room temperature overnight,Reaction to the material completely disappeared, dichloromethane extraction, concentration,Using a 5: 1 by volume petroleum ether: ethyl acetate column chromatography gradient elution,To give compound 10f; yield: 82% as a white solid

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 210532-25-5, its application will become more common.

Reference:
Patent; Shandong University; Liu Zhi; Chen Ting; Zhang Baojie; Feng Ying; Luo Xinyu; Cui Deliang; (19 pag.)CN106749315; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 102-49-8, name is 3,4-Dichlorobenzylamine, 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 102-49-8, SDS of cas: 102-49-8

General procedure: Triethylamine (0.3643 g, 3.6 mmol) was added to a solution of the appropriate alkylamine or substituted benzylamine 5a-l (3 mmol) in dichloromethane (7.5 mL), and the reaction mixture was stirred for 5 min at room temperature, then 2-chloroacetyl chloride (0.3857 g, 3.6 mmol) was added dropwise to this reaction mixture at 0 C and stirred for 15 min at room temperature. After completion of the reaction, the solvent was evaporated under reduced pressure to afford 6a-l. KI (0.5976 g, 3.6 mmol) and CTAB (98.40 mg, 7.5% mmol) were added to a solution of the crude product 6a-l in acetone (30 mL) and maintained stirring at reflux for 2 h to afford 7al. K2CO3 (0.2073 g, 3 mmol) was added to a solution of scopoletin (0.3843 g, 2 mmol) in acetone (30 mL), and the reaction mixture was stirred at refluxed for 30 min. Then crude intermediates 7a-l were added into the mixture and maintained reflux for 8-12 h (the reaction progress was monitored by TLC with UV detection). After cooling the reaction and filtration, the solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate, washed with saturation sodium bicarbonate, and saturation salt solution successively, dried over anhydrous sodium sulfate, evaporated under reduced pressure to give the target crude products. The crude products were purified by column chromatography using petroleum ether/ethyl acetate from 6:1 to 2:1 as the gradient eluent system to yield the products 26-37.

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, 3,4-Dichlorobenzylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Luo, Jinxiang; Lai, Ting; Guo, Tao; Chen, Fei; Zhang, Linli; Ding, Wei; Zhang, Yongqiang; Molecules; vol. 23; 5; (2018);,
Chloride – Wikipedia,
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Synthetic Route of 202197-26-0, These common heterocyclic compound, 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline, 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.

Example 6 4-[3-chloro-4-(3-fluoro-benzyloxy)-phenylamino]-6-nitro-quinazoline In a flask equipped with a reflux condenser, 6-nitro-4-chloro-quinazoline 1.20 g (5.7 mmol) and 4-(3-fluorobenzyloxy)-3-chloroaniline 1.37 g (5.6 mmol) were dissolved into 80 mL of isopropanol, and the solution was refluxed for 3 h. Then a lot of yellow solid was deposited, which was filtered, dried under vacuum, and identified as the title compound. Yield: 67%. 1H-NMR (400 MHz, CDCl3): delta11.30(1H, br), 9.54-9.48 (1H, m), 8.45-8.41 (1H, m), 8.31-8.25 (1H, m), 7.98-7.89 (1H, m), 7.50-7.47 (1H, m), 7.35-7.26 (1H, m), 7.05-6.96 (1H, m), 6.90-6.80 (2H, m), 7.74-7.60 (2H, m), 4.84 (2H, s).

The synthetic route of 202197-26-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SHANGHAI ALLIST PHARMACEUTICALS, INC.; US2008/300248; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 157590-59-5, 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. 157590-59-5, name is 4-Chloro-5-(trifluoromethyl)benzene-1,2-diamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

E. 6-Chloro-7-trifluoromethyl, 4-dihydro-2,3-quinoxalinedione A mixture of 3,4-diamino-6-chlorobenzotrifluoride (185 mg, 0.88 mmol) and oxalic acid dihydrate (117 mg, 0.93 mmol, used as received) in 2N HCl (4 mL) was refluxed at 170-5 C. for 3 h, then cooled to room temperature. The mixture was centrifuged and the liquid layer was removed. The yellow solid was washed twice by cold water (2*2 mL), collected by filtration, and dried at 60 C. with reduced pressure for 2 h, affording 180 mg of crude title compound (77.3%) as a light yellow powder. The crude product was dissolved in 1N NaOH (6 mL) and filtered. The filtrate was acidified to pH=6, affording 138 mg of title compound. It was recrystallized from DMSO/H2 O twice to give 102 mg of pure compound (43.9%) as yellow microcrystals. mp:>360 C. (dec. from 295 C.). IR (KBr, cm-1) 3425, 3200, 1731, 1706, 1625; 1400. 1 H NMR (DMSO-d6): delta7.274 (s, 1H); 7.478 (s, 1H); 12.145 (s, 2H). HRMS: calcd for C9 H4 ClF3 N2 O2 (M+) m/z: 263.9912; found: 263.9919.

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, 4-Chloro-5-(trifluoromethyl)benzene-1,2-diamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; The State of Oregon, acting by and through The Oregon State Board of Higher Education, acting for and on behalf of The Oregon Health Sciences University; The University of Oregon; The Regents of the University of California; US5514680; (1996); A;,
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. 367-22-6, name is 4-Chloro-3-fluoroaniline, A new synthetic method of this compound is introduced below., SDS of cas: 367-22-6

4-chloro-3-fluoroaniline (2g, 13.7 mmol) was dissolved in 60 mL of dichloromethane. Under ice bath, saturated sodium bicarbonate solution (60 mL) was added. The mixture was stirred at 0 C and triphosgene (1.36g, 4.58 mmol) was added. The mixture was stirred at 0 C for 1 hr and then extracted with dichloromethane and water. The organic layer was dried with sodium sulfate and filtered. The filtrate solution was concentrated and the residue was treated with 50 mL of hexanes. The hexane solution was concentrated to remove all solvents. The residue was dissolved in 12 mL of hexanes and filtered. The solution was concentrated and dried to give l-chloro-2-fluoro-4-isocyanatobenzene as an off white solid (1.69 g). 1H NMR (400 MHz, CHLOROFORM- )? ppm 6.82 – 6.90 (m, 1 H) 6.93 (dd, 7=9.22, 2.65 Hz, 1 H) 7.31 – 7.41 (m, 1 H).

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; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BROTHERTON-PLEISS, Christine E.; CHEN, Zhi; ERICKSON, Shawn David; KIM, Kyungjin; LI, Hongju; LOVEY, Allen John; QIAN, Yimin; SO, Sung-Sau; WOVKULICH, Peter Michael; YI, Lin; WO2014/60341; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 104-11-0,Some common heterocyclic compound, 104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, molecular formula is C8H10ClN, 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: The procedure is as follows: 3 mg of catalyst CoPz (hmdtn) 4 is weighed into a quartz jacketed photoreactor, and then 25 mL of a reaction solvent, acetonitrile (abbreviated as CH3CN), is added. CoPz(hmdtn)4 was completely dissolved in CH3CN under stirring. Further, 0.01 mmol of the auxiliary 1,8-diazabicycloundec-7-ene (abbreviated as DBU) and 1 mmol of N-methylbenzylamine were added to the above system. Stirring was continued for 2 h in the dark. Then, at 1 atm oxygen and lambda ? 420 nm visible light (using a xenon lamp as a light source, a 420 nm filter is used to filter out light having a wavelength of less than 420 nm, The following examples are the same as the light intensity of 1.01 W¡¤cm -2 ) for 3 h under light conditions. The reaction products were qualitatively analyzed and quantified by gas chromatography-mass spectrometry (GC-MS) and gas chromatography (GC). The experiment was recorded as Entry 1.

The synthetic route of 104-11-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; South Central University for Nationalities; Yang Changjun; Jin Juanjuan; Deng Kejian; Zhang Bingguang; (12 pag.)CN108623494; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics