Author: Jessica.F

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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2-Chloro-N,N-dimethylethanamine hydrochloride

To a mixture [OF 4-HYDROXYBENZALDEHYDE (1.] 34 g, 10.97 [MMOL)] and 2- dimethylaminoethyl chloride hydrochloride (1.95 g, 13.54 [MMOL)] in DMF (12 mL) was added KzCOs (6.04 g, 3.23 [MMOL).] The mixture was heated at reflux for 12 h. The residue was partitioned between [HZ0] and EtOAc. The organic layer was dried [(MGSO4),] filtered, and concentrated. The crude material was purified by flash chromatography [(10%] [MEOH/CH2CI2) TO YIELD 4-[2-(DIMETHYLAMINO) ETHOXYBENZALDEHYDE] (220 mg, 10%) as an orange liquid. ‘H NMR (400 MHz, CDCl3) 8 9. 87 (s, 1H), 7. [82 (D, 2H),] 7.01 (d, [2H),] 4.16 (t, [2H),] 2. [79 (T,] 2H), 2. 37 (s, 6H).

According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2004/9602; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 108-37-2, name is 1-Bromo-3-chlorobenzene, molecular formula is C6H4BrCl, 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 1-Bromo-3-chlorobenzene

To a stirred solution of 1-bromo-3-chlorobenzene (1.0 g, 5.22 mmol, 1.00 equiv) in tetrahydrofuran (5 mL), was added4,4,5 ,5-tetramethyl-2- (tetramethyl- 1 ,3,2-dioxaborolan-2-yl)- 1,3 ,2-dioxaborolane (800 mg, 3.15mmol, 0.60 equiv), 4-tert-butyl-2-(4-tert-butylpyridin-2-yl)pyridine (43 mg, 0.16 mmol, 0.03 equiv), bis(( 1Z,5Z)-cycloocta- 1 ,5-diene)dimethyl-2,4-dioxa- 1 ,3-diiridabicyclo[ 1.1 .0]butane-2,4-diium- 1 ,3-diuide (33 mg, 0.05 mmol, 0.01 equiv) under nitrogen. The mixture was stuffed for overnight at 80 C. The solid was filtered out and the filtrate was concentrated under vacuum. Crude product was purified by a silica gelcolumn with ethyl acetate/petroleum ether (1:10) to give 1.29 g (78%) of the title compound as colorless oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108-37-2, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; BLAQUIERE, Nicole; BURCH, Jason; CASTANEDO, Georgette; FENG, Jianwen A.; HU, Baihua; STABEN, Steven; WU, Guosheng; YUEN, Po-wai; WO2015/25025; (2015); A1;,
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, Quality Control of 3,4-Dichlorobenzylamine

General procedure: Compounds 5a?7a, 9a?11a, and 13a were synthetized using a microwave reactor with a focusedfield. Corresponding N-benzyl-3-chloropyrazine-2-carboxamide (0.6 mmol) was dissolved in methanol(3 mL) and appropriate benzylamine (1.8 mmol, 3 equiv.), along with pyridine (40 mg, 0.6 mmol,1 equiv.) as a base, were added. Our previous observations revealed that triethylamine (TEA) as a basecannot be used for microwave reactions. During the procedure, TEA is partially decomposed (probablyto diethylamine and similar species, which may act as undesired nucleophiles in the dehalogenationreaction). The use of pyridine as the base combined with benzylamines was experimentally verifiedin previous projects [18]. Conditions for synthesis were 150¡ãC, 30 min, and 100 W. The progressof the reactions was monitored by TLC in system hexane/ethyl acetate 1:1. The reaction mixturewas adsorbed on silica by removing the solvents in vacuo and the product was purified by flashchromatography using gradient elution with ethyl acetate (0?100percent) in hexane. Products 7a and 10awere recrystallized from EtOH/H2O.

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; Semelkova, Lucia; Jand’ourek, Ond?ej; Kone?na, Klara; Paterova, Pavla; Navratilova, Lucie; Trejtnar, Franti?ek; Kubi?ek, Vladimir; Kune?, Ji?i; Dole?al, Martin; Zitko, Jan; McPhee, Derek J.; Molecules; vol. 22; 3; (2017);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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,
Chlorides – an overview | ScienceDirect Topics

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