Category: chlorides-buliding-blocks

Application of 61881-19-4, The chemical industry reduces the impact on the environment during synthesis 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, I believe this compound will play a more active role in future production and life.

General procedure: To an ice cooled suspension of NaH (3.3mmol) in dry THF (20mL) under nitrogen atmosphere was slowly added a solution of the ketone 8a-e(1mmol) in THF (5mL). The resulting suspension was stirred for 30min at 0C and then a solution of the corresponding trifluoroacetimidoyl chloride 9a-e (1mmol) in dry THF (3mL) was slowly added dropwise at 0C and then further stirred at room temperature for 3h. The resulting orange-brown solution was evaporated under reduced pressure, water was added carefully (20mL) and extracted with CHCl3 (2×20mL). The organic extract was separated, dried over anhydrous magnesium sulfate and evaporated obtaining a brown oil, which was further purified either by recrystallization or column chromatography (silicagel, Hex 7: EtOAc 3).

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, 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Romero, Angel H.; Salazar, Jose; Lopez, Simon E.; Journal of Fluorine Chemistry; vol. 169; (2015); p. 32 – 37;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 95-81-8, The chemical industry reduces the impact on the environment during synthesis 95-81-8, name is 2-Chloro-5-methylaniline, I believe this compound will play a more active role in future production and life.

Reference Example 12 4-Chloro-6-(2-chloro-5-methylanilino)pyrimidine Tetramethylene sulphone (10 ml) was added to 4,6-dichloropyrimidine (25.0 g, 170 mmol) and heated to 125 C. 2-Chloro-5-methylaniline (11.90 g, 84 mmol) was added portion wise over 20 mins. The reaction mixture was heated at 125 C. for 2 hours. The reaction was allowed to cool to room temperature and DCM (200 ml) was added. The mixture was basified to pH 9-10 with methanolic ammonia and evaporated onto silica (15 g). The residue was purified by column chromatography eluding with EtOAc:isohexane (10:90) to give a white solid (12.25 g, 29%). NMR (300 MHz): 2.3 (s, 3H), 6.7 (s, 1H), 7.0 (d, 1H), 7.4 (d, 1H), 7.5 (s, 1H), 8.4 (s, 1H), 9.4 (s, 1H); m/z 254 (MH+).

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-5-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AstraZeneca AB; US6632820; (2003); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 26487-67-2, name is 1-(2-Chloroethyl)azepane 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 26487-67-2, Recommanded Product: 26487-67-2

Example 7 1-(2-(1-Perhydroazepinyl)ethyl)-3,4-dimethyl-4-(3-(1H-1,2,3-triazol-4-yl)phenyl)piperidine A solution of 1-(2-chloroethyl)perhydroazepine hydrochloride (42 mg, 0.21 mmol) in N,N-dimethylformamide (1 mL) was treated with triethylamine (30 muL, 0.22 mmol) then transferred to a flask containing 3,4-dimethyl-4-(3-(1H-1,2,3-triazol-4-yl)phenyl)piperidine (Preparation 44, 45 mg, 0.176 mmol) in N,N-dimethylformamide (2 mL). Sodium iodide (32 mg, 0.21 mmol) and sodium hydrogencarbonate (18 mg, 0.21 mmol) were added and the resultant mixture was heated at 60°C overnight. The solvent was then removed in vacuoand the residue was partitioned between saturated aqueous sodium hydrogencarbonate solution (5 mL) and dichloromethane (5 mL). The phases were separated and the aqueous layer was further extracted with dichloromethane (2 x 5 mL). The combined extracts were dried over Na2SO4, filtered and concentratedin vacuo.The residue was purified by reversed phase preparative HPLC (condition 2) to give the acetate salt of the title compound. The free base was obtained by treating with dilute aqueous ammonia solution (2 mL) and extracting with ether (4 x 3 mL). Drying over Na2SO4, filtering andevaporation to dryness gave the title compound as a white solid (16 mg, 24percent). NMR (CDCl3, selected data for the free base): 0.8 (d, 3H), 1.35 (s, 3H), 1.6-1.8 (m, 9H), 2.10 (m, 1H), 2.4-2.5 (m, 2H), 2.6-3.0 (m, 11H), 7.25 (d, 1H), 7.35 (t, 1H), 7.55 (d, 1H), 7.85 (s, 1H), 7.95 (s, 1H). MS (thermospray): M/Z (MH+) 382.6; C23H35N5+ H requires 382.3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(2-Chloroethyl)azepane hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; PFIZER INC.; Pfizer Limited; EP1072601; (2001); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 14862-52-3,Some common heterocyclic compound, 14862-52-3, name is 3,5-Dibromochlorobenzene, molecular formula is C6H3Br2Cl, 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.

In the round bottom flask was charged with 1,3-dibromo-5-chlorobenzene 25g (92.47mmol) and methyl diphenyl amine 33.9g (184.9mmol) into a sodium t- butoxide 26.7g (277.41mmol) was added to 463ml toluene dissolved. Here Pd (dba)2 0.266g (0.462mmol) and tri-tert-butylphosphine was put 0.187g (0.924mmol) in turn and the mixture was stirred under reflux for 4 hours under a nitrogen atmosphere. After the reaction the organic layer was then extracted with ethyl acetate dry distilled over magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The product n- hexane / dichloromethane (9: 1 by volume) to yield the silica gel column 37.3g (yield 85%) of intermediate M-11 the desired compound is purified by chromatography 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 3,5-Dibromochlorobenzene, its application will become more common.

Reference:
Patent; Chei Industries Inc.; Ryu, Dong Wan; Heo, Dal Ho; Jung, Seong Hyeon; Hong, Jin Seok; Kim, Jun Seok; Yoo, Dong Kyu; Lee, Seung Jae; Lee, Han Il; Chang, Yu Na; Cho, Yeong Kyeong; Chae, Mi Yeong; (44 pag.)KR2016/8651; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 210532-25-5, 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. 210532-25-5 name is 3,5-Difluorobenzene-1-sulfonyl chloride, 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.

1.132 g (5.32 mmol) of 3,5-dif uorobenzene-l-sulfonyle chloride is added under argon to a solution of 545 mg (3.55 mmol) of 5-amino-2-chloronicotinotrile in 20 mL of an anhydrous 1 : 1 mixture of THF and pyridine. The reaction medium is heated to 70C for 3 hours and let 12 additional hours under stirring at room temperature. The solvent is dry evaporated and the crude reaction product is redissolved in ethyl acetate and washed with several aqueous fractions. The organic phase is dried on magnesium sulfate, filtered, concentrated and then purified by silica gel chromatography to yield 784 mg (67%) of N-(6-chloro-5-cyanopyridin-3-yl)-3,5-difluorobenzene-sulfonamide.1H NMR: deltaEta ppm (400 MHz, DMSO) : 1 1,39 (1H, si, NH), 8. 34 (1H, m, CHarom), 8, 10 (1H, m, CHarom), 7,67 (1H, m, CHarom), 7,59 (2H, m, CHarom).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Difluorobenzene-1-sulfonyl chloride, and friends who are interested can also refer to it.

Reference:
Patent; PIERRE FABRE MEDICAMENT; KALOUN, El Bachir; BEDJEGUELAL, Karim; RABOT, Remi; KRUCZYNSKI, Anna; SCHMITT, Philippe; PEREZ, Michel; RAHIER, Nicolas; WO2012/101239; (2012); A1;,
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. 367-21-5, name is 3-Chloro-4-fluoroaniline, A new synthetic method of this compound is introduced below., COA of Formula: C6H5ClFN

To a stirred solution of 3-chloro-4-fluoroaniline (Tokyo Chemical Industry, 5.00 g, 34.4 mmol) and dry pyridine (3.50 mL, 43.3 mmol) in dry CH2Cl2 (17.0 mL) was added dropwise a solution of bromine (1.90 mL, 36.9 mmol) in CH2Cl2 (10.0 mL) at 0 C under N2. The reaction mixture was stirred at the temperature under N2 for 1 h, warmed up to room temperature, and stirred for 1 h. The mixture was poured into H2O and then extracted with AcOEt. The extracts were dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography (silica gel, hexane/AcOEt = 10:1) to afford 2.76 g of the title product 18 in 36% yield as a brown solid. 1H NMR (270 MHz, CDCl3) delta 7.22 (1H, d, J = 8.6 Hz), 6.77 (1H, d, J = 6.4 Hz), 3.84 (2H, br s).

The synthetic route of 367-21-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hayashi, Shigeo; Ueno, Naomi; Murase, Akio; Nakagawa, Yoko; Takada, Junji; European Journal of Medicinal Chemistry; vol. 50; (2012); p. 179 – 195;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 60633-25-2, name is 2-Bromo-4-chloro-1-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H6BrClO

Heat a mixture of commercially available 2-bromo-4-chloro-1-methoxybenzene (8.0 g, 36.1 mmol, ), phenol (6.80 g, 72.2 mmol), cesium carbonate (23.54 g, 72.2 mmol), copper (I) chloride (1.79 g, 18.1 mmol) and 2,2,6,6-tetramethyl-3,5-heptanedione (1.66 g, 9.00 mmol) in n-methyl-2-pyrrolidinone (80 mL) at 120 C for 20 h. Cool to room temperature, filter and quench the filtrate with 1 N hydrochloric acid (SO mL). Dilute the filtrate with diethyl ether and extract with water. Dry (sodium sulfate), concentrate and purify (silica gel chromatography, eluting with 90: 10 hexanes: ethyl acetate) to give the title compound 7.42 g (88%).- ¹H NMR (400 MHz, CDCl3) No. 7.35-7.27 (m, 2 H), 7.12-7.05 (m, 2 H), 6.98-6.95 (m, 2 H), 6.93-6.89 (m, 2 H), 3.85 (s, 3 H)

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 60633-25-2.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/100301; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 33786-89-9, name is 5-Chloro-m-phenylenediamine, This compound has unique chemical properties. The synthetic route is as follows., category: chlorides-buliding-blocks

A suspension of 2,6-dichloro-9-isopropyl-9H-purine (3.0 g, 12 mmol) and 5-chlorobenzene-1,3-diamine (1.8 g, 12 mmol) in n-butanol (21 mL) was stirred at rt as DIPEA (4.1 mL, 24 mmol) was added drop-wise. The resulting suspension was allowed to stir at 100 C and the suspension became a clear solution. After 8 h heating, the solution became a suspension. This suspension was allowed to cool to rt and filtered. The solids were washed with EtOAc (2×10 mL) and dried under vacuum. The title compound (3.6 g) was recovered as solid in 83% yield. 1H NMR (399 MHz, DMSO-d6) delta 10.08 (s, 1H), 8.42 (s, 1H), 7.10 (t, J = 1.9 Hz, 1H), 6.96 (t, J = 1.9 Hz, 1H), 6.33 (t, J = 2.0 Hz, 1H), 5.41 (s, 2H), 4.71 (p, J = 6.8 Hz, 1H), 1.51 (d, J = 6.7 Hz, 6H); 13C NMR (75 MHz, DMSO-d6) delta 152.7, 152.3, 150.7, 150.6, 141.0, 140.9, 133.4, 119.6, 109.2, 108.9, 105.4, 47.4, 22.6, 22.5; HRMS (ESI) m/z calcd for C14H14Cl2N6 (M + H)+, 337.0730; found, 337.0727.

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 33786-89-9.

Reference:
Article; Shi, Yihui; Park, Jaehyeon; Lagisetti, Chandraiah; Zhou, Wei; Sambucetti, Lidia C.; Webb, Thomas R.; Bioorganic and Medicinal Chemistry Letters; vol. 27; 3; (2017); p. 406 – 412;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 7006-52-2, 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. 7006-52-2, name is N-Methyl-3-chloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3-Chloro-N-methylaniline (0.47 mL, 3.90 mmol) and anhydrous NaHCO3 (1.94 g) were ground together into fine powder, and commercially available benzenesulfonylchloride 6 (915 mg, 3.88 mmol) was added under vigorous stirring at room temperature. The progress of reaction was monitored by TLC until the conversion of amine was completed. After 30 min., the reaction mixture was diluted with water, acidified with 1N aqueous HCl, extracted several times with Et2O and the combined organic phase was dried over anhydrous sodium sulphate. Evaporation under vacuum of the organic solvent afforded a crude product corresponding to the sulfonamidic derivative.

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, N-Methyl-3-chloroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Granchi, Carlotta; Roy, Sarabindu; Mottinelli, Marco; Nardini, Elisa; Campinoti, Fabio; Tuccinardi, Tiziano; Lanza, Mario; Betti, Laura; Giannaccini, Gino; Lucacchini, Antonio; Martinelli, Adriano; MacChia, Marco; Minutolo, Filippo; Bioorganic and Medicinal Chemistry Letters; vol. 21; 24; (2011); p. 7331 – 7336;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 3972-56-3, The chemical industry reduces the impact on the environment during synthesis 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene, I believe this compound will play a more active role in future production and life.

General procedure: To a 30 ml of two necked flask, Pd catalyst, HCO2M (M: H, Na, K),Base (Cs2CO3, K2CO3, Na2CO3, Et3N), X-C6H4-R (1 mmol) and 2,5-norbornadiene were introduced. 5 ml of solvent (DMF, DMA,DMSO) was added to the mixture under nitrogen. The resultant mixture was heated at 120 °C and stirred for 4~7 hours. The mixture was cooled to ambient temperature and poured into 30 ml of water. The combined mixture was extracted with ether (50ml, 3 times). The organic layer was washed with water and brine.The washed organic layer was dried over MgSO4, filtered and condensed in vacuo. The residue was analyzed via GC quantitatively, using internal standard. Also the residue was chromatographed on SiO2 with hexane – ethyl acetate. The purified compound was determined its chemical structure with NMR analysis.

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-tert-Butyl-4-chlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Aida, Fuyuki; Sone, Hisashi; Ogawa, Ryuhei; Hamaoka, Takeharu; Shimizu, Isao; Chemistry Letters; vol. 44; 5; (2015); p. 715 – 717;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics