Month: May 2021

Reference of 29027-17-6, The chemical industry reduces the impact on the environment during synthesis 29027-17-6, name is 2-Chloro-3-methylaniline, I believe this compound will play a more active role in future production and life.

a (2-Chloro-3-methyl-phenyl)-hydrazine The title compound was prepared in accordance with the general method of example 25a) from 2-chloro-3-methylaniline.

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-Chloro-3-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bentley, Jonathan M.; Hebeisen, Paul; Muller, Marc; Richter, Hans; Roever, Stephan; US2002/35110; (2002); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 121-27-7, These common heterocyclic compound, 121-27-7, name is 5-Chloro-2-(4-chlorophenoxy)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.

A mixture of 43.6 g. of isonicotinic acid, 200 ml. of thionyl chloride and 200 ml. of methylene chloride is heated under reflux for 2 hours. The solvent is evaporated, 93.4 g. of 5-chloro-2-(p-chlorophenoxy)aniline, 180.0 g. of anhydrous potassium carbonate and 2800 ml. of benzene are added and the reaction proceeds as described in Example 1. Extraction with petroleum ether gives 5′-chloro-2′-(p-chlorophenoxy)-isonicotinanilide.

The synthetic route of 121-27-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; American Cyanamid Company; US4221714; (1980); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 179897-90-6,Some common heterocyclic compound, 179897-90-6, name is 1,3-Dibromo-2-chloro-5-fluorobenzene, molecular formula is C6H2Br2ClF, 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 round bottom flask under nitrogen fitted with a stir bar was added 1- chloro-2,6-dibromo-4-fluorobenzene (14.36 g, 49.8 mmol), pivalamide (5.04 g, 49.8 mmol), cesium carbonate (21.09 g, 64.7 mmol) and dioxane (250 mL). The reaction mixture was sparged with nitrogen and Pd(dba)2 (1.43 g, 2.490 mmol) and 5-bis(diphenylphosphino)-9,9- dimethylxanthene (XANTPHOS, 2.02 g, 3.49 mmol) were added. The reaction was then sealed and heated in an oil bath at 70 C for 18 h. The reaction was allowed to cool to r.t and was partitioned between a saturated aqueous solution of NH4C1 and EtOAc. The layers were separated and the aqueous portion was extracted with EtOAc (2 X). The combined organic portions were washed with water, brine, dried (Na2S04), filtered, concentrated, and adsorbed onto silica gel. Purification by flash chromatography on silica gel using an EtO Ac- heptane (1-20%) elution gradient afforded N- (3-bromo-2-chloro-5-fluorphenyl)pivalamide (1 1.0 g, 33.8 mmol, 68 %) as a white crystalline solid. LCMS (m/z): 309.9 (MH+), tR = 1.1 1

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dibromo-2-chloro-5-fluorobenzene, its application will become more common.

Reference:
Patent; NOVARTIS AG; MADERA, Ann Marie; POON, Daniel; SMITH, Aaron; WO2011/161216; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 41332-02-9,Some common heterocyclic compound, 41332-02-9, name is 1-(2-Chloroethyl)naphthalene, molecular formula is C12H11Cl, 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: An aqueous solution of [18F]F- (0.5-3.5 mL, flow rate 0.5-30 mL/min) was passed through the column (borosilicate glass tubing, ID 4 mm, OD 0.6 cm, length 12 cm) packed with the resin (5-500 mumol; glass beads to fill the remaining volume). To remove the bulk of water, the column was flushed with He(gas) (flow rate 100 mL/min, 3 min). The column was dried by passing MeCN oracetone (1-10 mL, flow rate 1.5-20 mL/min) through, followed by a helium flush (100 mL/min,2-5 min). The column was primed by passing the radiofluorination solvent (MeCN for mannosetriflate, MeCN/tBuOH 1:5 for FLT-ONs, toluene for the naphthalene derivatives and 2-nitro-3-methoxypyridine, dry, 4 mL, flow rate 2 mL/min) through the column at room temperature followed by the substrate (50-100 mumol) dissolved in the radiofluorination solvent (dry, 3 mL) at 60-120 C (flow rate 0.55 mL/min). The radiofluorination solvent (dry, 2 mL, flow rate 0.55 mL/min) was then passed through the column again to elute the remaining product. The reaction mixture was analyzed by radio-TLC (eluent heptane:EtOAc 80:20 for the naphthalene derivatives, MeCN:H2O 95:5 for FDG, DCM:MeOH 9:1 for hydrolyzed FLT, petroleum ether:EtOAc 3:1 for the pyridine derivative. Total timeof radiosynthesis was 35-45 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(2-Chloroethyl)naphthalene, its application will become more common.

Reference:
Article; Mathiessen, Bente; Zhuravlev, Fedor; Molecules; vol. 18; 9; (2013); p. 10531 – 10547;,
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. 54773-20-5, name is 1,3-Dichloro-5-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Quality Control of 1,3-Dichloro-5-(trifluoromethyl)benzene

PREPARATION 1 1-(3-Chloro-5-trifluoromethyl-phenyl)-piperazine Beginning with 3,5-dichlorobenzotrifluoride (500 mg, 2.32 mmol) and piperazine (1 g, 11.6 mmol), 320 mg of the title compound was recovered by the procedure described in Example-1.

The synthetic route of 54773-20-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sonesson, Clas; Andersson, Bengt; Waters, Susanna; Waters, Nicholas; Tedroff, Joakim; US2003/4169; (2003); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 6480-66-6,Some common heterocyclic compound, 6480-66-6, name is 2,6-Dichloro-4-methoxyaniline, molecular formula is C7H7Cl2NO, 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.

Trichloromethyl carbonochloridic acid ester (0.0065 mol) was added to the solution of 2,6-dichloro-4-methoxybenzenamine (0.001 mol) and Et3N (0.4 ml) in dry toluene (16 ml). The reaction mixture was stirred for 2 hours at 6O0C till the starting aniline reacted completely (control by TLC). Then, a solution of intermediate 24 (prepared according to A8.c) in DCM (4 ml) was added to the reaction mixture at 6O0C at stirring. Formation of precipitate was observed. The stirring was continued at 60-70C for 1 hour. Then, the reaction mixture was concentrated in vacuum. The formed sediment was treated with water and filtered off. Then, it was washed with water, ethyl acetate, ether, and dried on the air. Yield: 0.360 g of compound 15 (66 %).

The synthetic route of 6480-66-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2008/148868; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 90390-33-3, 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. 90390-33-3 name is 3-Chloro-5-fluorobenzylamine, 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.

Weigh 159 mg of 3-chloro-5-fluorobenzylamine (1 mmol) in a dry 50 mL eggplant-shaped reaction flask, add 15 mL of dichloromethane, and stir until the substrate is completely dissolved.After adding 200 muL of triethylamine, 192 mg of (E) oct-6-enoyl chloride (1.2 mmol) dissolved in an appropriate amount of dry dichloromethane) was slowly added dropwise under an ice bath at 0 to 5 C.After the completion of the dropwise addition, the TLC tracking and monitoring were carried out at room temperature, and when the raw materials disappeared, 20 mL of saturated sodium hydrogencarbonate was sequentially used.The water and the saturated aqueous NaCl solution were each washed three times and dried over anhydrous sodium sulfate.The mixture was separated by silica gel column chromatography under reduced pressure to give (E)-N-(3-chloro-5-fluorobenzyl)oct-6-enamide.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-5-fluorobenzylamine, and friends who are interested can also refer to it.

Reference:
Patent; Shanghai Shidande Biological Co., Ltd.; Shanghai Shidande Criterion Technology Services Co., Ltd.; Qian Yong; Xin Zhenqiang; Shu Yaping; Zhang Tianyong; Xie Tianpei; (11 pag.)CN108503559; (2018); 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. 200190-87-0, name is 1-Bromo-4-chloro-2-fluoro-5-methylbenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Bromo-4-chloro-2-fluoro-5-methylbenzene

(2) Ether solution (45mmol) containing the compound prepared by the method of the Reference Example 9 (1) (3.15g, 14mmol) was stirred at -78?C, followed by dropwise addition of n-butyl lithium (1.6M in hexane, 10.2ml, 16mmol) over 10 minutes, and the stirring was continued at the same temperature for 30 minutes. Then, trimethyl borate (1.77g, 17mmol) in ether (8ml) was dropwise added at the same temperature over 10 minutes, and the resulting mixture was stirred for 3 hours at the same temperature. The temperature of the mixture was gradually increased to the room temperature by standing overnight. 1N hydrochloric acid (50ml) was added with ice cooling and the mixture was stirred at room temperature for 1 hour. The ether layer was separated, and the aqueous layer was extracted with ether. The ether layers were combined, washed with brine, dried and concentrated by evaporation of the solvent. A small amount of petroleum ether was added to the residue, followed by filtration of deposited crystals. The crystals were dried to obtain 4-chloro-2-fluoro-5-methylphenylboronic acid (2.94g). m.p.250-253?C 1H-NMR(DMSO-d6) delta 2.29(3H, s), 7.23(1H, d, J=8.8Hz), 7.50(1H, d, J=6.6Hz), 8.23(2H, br s) 19F-NMR(DMSO-d6) delta -106.1 IR(Nujol) 3360, 1608, 1568, 1235, 1132, 1045, 944, 795 cm-1

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; Sumitomo Chemical Takeda Agro Company, Limited; EP1333029; (2003); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 202865-57-4, name is 1-Bromo-2,5-dichloro-3-fluorobenzene, 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 202865-57-4, Safety of 1-Bromo-2,5-dichloro-3-fluorobenzene

6-chloro-2-fluoro-3-methylphenol (3.3 g, 20.55 mmol) and 18-crown-6 (1.086 g, 4.11 mmol) were dissolved in dry DMSO (50 ml.) and treated with 20% potassium t- butoxide in THF (1 1.50 g, 20.55 mmol) for 15 minutes at room temperature. 1- bromo-2,5-dichloro-3-fluorobenzene (7.21 g, 29.6 mmol) was added in one portion and the reaction mixture heated at 1 100C for 3 days at which time LC-MS indicated nearly complete consumption of phenol and formation of a major new product. Addition of water to the reaction mixture resulted in a brown gummy oil which was extracted with EtOAc. The organic phase was isolated, washed with brine four times, dried over MgSOphi filtered and concentrated to dryness to give a brown syrup. This material was filtered through a plug of 45 g silica gel which was eluted with 500 ml_ DCM. The filtrate was concentrated to an amber oil and crystallized from EtOH and a few drops of water. This mixture was cooled in an ice bath, filtered, and the precipitate washed with three portions of cold EtOH to give 2-[(3-bromo-2,5- dichlorophenyl)oxy]-1-chloro-3-fluoro-4-methylbenzene (4.0 g, 10.40 mmol, 50.6 % yield) as a cream solid. 1 H NMR (400 MHz, DMSO-c/6) delta ppm 7.73 (s, 1 H), 7.29 – 7.47 (m, 2 H), 6.81 (s, 1 H), 2.29 (s, 3 H).

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; SMITHKLINE BEECHAM CORPORATION; WO2008/154271; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 127049-87-0, The chemical industry reduces the impact on the environment during synthesis 127049-87-0, name is 1-Bromo-2,4-dichloro-3-methylbenzene, I believe this compound will play a more active role in future production and life.

Treat a mixture of 1-bromo-2,4-dichloro-3-methyl-benzene (76.01 g, 0.316 mol) and N-bromosuccinimide (59.2 g, 0.332 mol) in CCl4 (500 mL) with benzoyl peroxide (0.77 g, 3.18 mmol) and is heat to reflux for 6 hours under N2. Cool the reaction mixture to 0 C. and filter using hexanes to rinse the solids. Extract the filtrate with water and saturated NaHCO3. Dry the organic layer (Na2SO4) and remove the solvent in vacuo to afford 97.89 g (97%) of the titled product. Rf=0.34 (100% hexanes).

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-2,4-dichloro-3-methylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Aicher, Thomas Daniel; Anzeveno, Peter Biagio; Li, Renhua; Krasutsky, Alexei Pavlovych; Mabry, Thomas Edward; Saeed, Ashraf; Snyder, Nancy June; Stephenson, Gregory Alan; Tian, Hongqi; Wallace, Owen Brendan; Winneroski, JR., Leonard Larry; Xu, Yanping; US2009/111800; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics