Tag: M.W=100-200

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 2613-30-1 as follows. HPLC of Formula: C6H4ClF2N

Anhydrous copper (II) bromide (2.7 g, 12.1 mmol) and t-butyl nitrite (1.56 g, 15.1 mmol) were combined in anhydrous acetonitrile (25 mL). The resulting mixture was heated to 65 C. and a solution of 4-chloro-2,5-difluoro-phenylamine (1.65 g, 10.1 mmol) in anhydrous acetonitrile (2 mL) was added dropwise (vigorous gas evolution was noted). After the reaction mixture cooled to ambient temperature, it was added to 2N HCl and extracted twice with diethyl ether. The organic extracts were then combined, washed with 2N HCl, washed with saturated sodium bicarbonate, dried, concentrated and purified by flash chromatography on silica gel (hexanes) to give the title compound as a white solid (1.11 g, 48.4% yield): 1H NMR (CDCl3) delta 7.38 (dd, 2H), 7.21 (dd, 2H).

According to the analysis of related databases, 2613-30-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Dow AgroSciences LLC; US2009/88322; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 94-97-3, These common heterocyclic compound, 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, 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.

General procedure: A 35-mL Schlenk tube, equipped with a magnetic stirring bar, was charged with 9H-xanthene 1a (137 mg, 0.75 mmol), 1H-benzo[d][1,2,3]triazole 2a (60 mg, 0.5 mmol), and BPO (242 mg, 1.0 mmol), followed by the addition of DCE (5.0 mL). The mixture was stirred at 80 C for 6 h; then it was quenched with saturated aqueous Na2S2O3 (2.0 mL), saturated aqueous K2CO3 (2.0 mL), and water (20.0 mL), and extracted with CH2Cl2 (20.0 mL) three times. The residue obtained after evaporation of the solvent was purified by column chromatography on silica gel (petroleum ether/ethyl acetate = 12:1, v/v) to afford 1-(9H-xanthen-9-yl)-1H-benzo[d][1,2,3]triazole 3a as a colorless crystal (144 mg, 96% yield).

Statistics shows that 5-Chloro-1H-benzo[d][1,2,3]triazole is playing an increasingly important role. we look forward to future research findings about 94-97-3.

Reference:
Article; Li, Yanni; Li, Yanping; Li, Yuan; Chen, Chunlin; Ying, Fengyuan; Dong, Ying; Liang, Deqiang; Synthetic Communications; vol. 49; 16; (2019); p. 2053 – 2065;,
Chloride – Wikipedia,
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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

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,
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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;,
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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

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

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