Month: July 2021

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. 2163-00-0, name is 1,6-Dichlorohexane, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C6H12Cl2

EXAMPLE 2A 1,6-Bis(4-cyanomethylmorpholinium)hexane Dichloride (HDMMA) 100 ml of morpholine (1.147 mole) and 150 ml ethylacetate (EtOAc) were added to 500 ml Morton flask equipped with reflux condenser, thermometer, mechanical stirrer, and heating mantel. 25 ml of 1,6-dichlorohexane (0.172 mole) was added slowly to flask at room temperature. This was refluxed for 48 hours. Gas chromatogram showed 90% completion of the reaction. The product 1,6-bismorpholinohexane was purified from reaction mixture by vacuum filtration to remove the morpholine hydrochloride, and the light yellow filtrate was purified by adsorption chromatography. 13 C NMR showed a spectrum consistent with structure with very minor impurities. Gas chromatography showed an approximate purity of 98.2% based upon peak areas. The collected amount of 1,6-bismorpholinehexane was 30.0 g, which corresponds to a yield of 66.6%.

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 2163-00-0.

Reference:
Patent; The Clorox Company; US5739327; (1998); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 4535-90-4,Some common heterocyclic compound, 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, molecular formula is C3H9Cl2N, 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.

(ii) The white crystal 3 (1.0 g, 7.69 mmol) and sodium thiosulfate pentahydrate (1.91 g, 7.69 mmol) were added into 100 mL flask. MilliQ water (10 mL) was then added into the flask, and the reaction mixture was stirred at 120 C for 24 h under argon atmosphere. The reaction was then cooled to room temperature and the solvent was removed under reduced pressure. Hydrochloric acid (6.0 M, 25 mL) was added into the flask and the solution was stirred at 85 C for 3 h under argon atmosphere. The solvent was then removed, and 100 mL of dichloromethane and 15 mL of ethanol were added to extract the product. Sodium chloride and sulfate salts were precipitated from the solution. The salts were then filtered and the filtrate was concentrated to give product as a white solid (0.55 g, yield: 56.1%). The B monomer was extremely hygroscopic, which was needed to be stored in a dry oven. The 1H NMR and 13C NMR spectra of B monomer were shown in Fig. S4.

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

Reference:
Article; Xu, Chao-Ran; Zhang, Ze; Pan, Cai-Yuan; Hong, Chun-Yan; Polymer; vol. 172; (2019); p. 294 – 304;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 108-37-2, A common heterocyclic compound, 108-37-2, name is 1-Bromo-3-chlorobenzene, molecular formula is C6H4BrCl, 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 flask containing (l,5-cyclooctadiene)(methoxy)-iridium(I) dimer (84 mg, 0.13 mmol), 4,4′-di-tert butyl-2-2′-dipyridyl (69 mg, 0.26 mmol) and bis(pinacolato)diboron (1.29 g, 5.11 mmol) was purged with Ar, then hexanes (26 mL) and l-bromo-3- chlorobenzene (1 mL, 8.51 mmol) were added sequentially. The solution was stirred at RT for 18 h. The reaction mixture was concentrated in vacuo, re-dissolved in acetone (26 mL), then oxone (5.23 g, 8.51 mmol) in water (26 mL) added [Caution: exotherm observed]. After 10 min, the reaction mixture was diluted with DCM. The layers separated, and the aqueous layer extracted with DCM. The combined organics were washed with brine, dried and concentrated in vacuo to give the title compound (1.43 g, 81%). LCMS (Method 3): Rt 3.74 min, m/z 205, 207 [M-H+].

The synthetic route of 108-37-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHIESI FARMACEUTICI S.P.A.; ALCARAZ, Lilian; HURLEY, Christopher; CRIDLAND, Andrew, Peter; JENNINGS, Andrew, Stephen, Robert; WO2014/195402; (2014); 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. 93765-83-4, name is 1-Bromo-5-chloro-2-fluoro-4-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H5BrClF

A mixture of 1-bromo-5-chloro-2-fluoro-4-methylbenzene (500 mg, 2.3 mmol), N-bromosuccinimide (481 mg, 2.7 mmol) and azobisisobutyronitrile (38 mg, 0.23 mmol) in CCl4 (10 mL) was stirred at 90 C for 16 h. The mixture was diluted with DCM (20 ml) and water (20 ml). The organic layer was separated, dried over Na2S04, filtered and evaporated to get crude product. The residue was purified by silica column chromatography (eluting with petroleum ether/ethyl acetate = 50/1) to give 1-bromo-4-(bromomethyl)-5-chloro-2-fluorobenzene as a solid (324 mg, 47%).

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 93765-83-4.

Reference:
Patent; GENENTECH, INC.; XENON PHARMACEUTICALS INC.; CHEN, Chien-An; CHOWDHURY, Sultan; DEHNHARDT, Christoph Martin; SUN, Shaoyi; WO2014/144545; (2014); A2;,
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

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

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

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

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

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