Month: June 2021

Related Products of 694-80-4, 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. 694-80-4 name is 1-Bromo-2-chlorobenzene, 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.

General procedure: To a round bottle with a magnetic stir bar, ligand (0.01% mmol), PdCl2 (0.01% mmol), aryl halides (1.0 mmol), phenylboronic acid (1.2 mmol), K2CO3 (2.0 mmol) and 6 ml of solvent were added. The reaction mixture was conducted at room temperature for the required time, and then the solvent was removed under reduced pressure. The residual was diluted with Et2O (5 mL), followed by extraction twice (2×5 mL) with Et2O. The organic layer was dried with anhydrous MgSO4, filtered and evaporated under vacuum. The conversions rates were analyzed by gas chromatography, based on the peak area normalization method. The corrected factor was determined by samples against a standard of n-heptane. The crude products were purified by silica-gel column chromatography using petroleum ether-ethyl acetate (20:1) as an eluent, and the isolated yield was then calculated based on the feeding of the aryl halide. The isolated corresponding products were characterized by 1H NMR and 13C NMR.

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

Reference:
Article; Zhou, Zhen; Cao, Gao; Liu, Ning; Chemistry Letters; vol. 48; 6; (2019); p. 547 – 550;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 13078-80-3,Some common heterocyclic compound, 13078-80-3, name is 2-(2-Chlorophenyl)ethanamine, molecular formula is C8H10ClN, 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 1 Into a 100 ml reaction flask equipped with a condenser, a thermometer and a stirrer, 15.56 g (0.1 mol) of 2-chlorophenethylamine, 22.0 g (0.11 mol) of a 20% sodium hydroxide aqueous solution and 0.176 g (0.5 mol %) of quinoline copper were charged, and reacted at 110 C. for 8 hours. The reaction mixture thereby obtained was subjected to liquid separation to separate the aqueous layer from the organic layer. The organic layer was washed with an acid and distilled to obtain 11.4 g of indoline (boiling point: 94-95 C./11 mmHg). The purity was 99.5%, and the yield was 96%.

The synthetic route of 13078-80-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ihara Chemical Industry Co., Ltd.; US4673749; (1987); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 2401-24-3, 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. 2401-24-3, name is 2-Chloro-5-methoxyaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

6-(benzyloxy)-3-bromo-2-methylpyridine (ArkPharm catalog No.AK-27978, 0.1 g, 0.360 mmol), 2-(dicyclohexylphosphino)-2′,4′,6′-tri-1-propyl-1,1′-biphenyl (Chemimpex catalog No.27675, 0.013 g, 0.027 mmol), cesium carbonate (0.141 g, 0.431 mmol) and palladium (II) acetate (4.04 mg, 0.018 mmol) were added to a microwave vial containing a stir bar and 5 mL of anhydrous toluene. Then, 2-chloro-5-methoxyaniline (Chemimpex catalog No.27675, 0.059 g, 0.378 mmol) was added. The solvent was degassed with argon twice. The reaction was heated on a heating block to 100 C. for 15 hours. The crude reaction mixture was cooled to room temperature and then filted through celite. The celite was rinsed repeatedly with ethyl acetate to collect the crude product mixture. A normal phase ethylacetate/hexanes column was run on the crude mixture to give 6-(benzyloxy)-N-(2-chloro-5-methoxyphenyl)-2-methylpyridin-3-amine (0.1195 g, 94% yield). 1H NMR (CDCl3, 400 MHz) delta 7.39 (m, 6H), 7.20 (d, 1H, J=8.8 Hz), 6.67 (d, 1H, J=8.4 Hz), 6.26 (dd, 1H, J=2.8, 8.8 Hz), 6.01 (d, 1H, J=2.8 Hz), 5.65 (s, 1H), 5.37 (s, 2H), 3.65 (s, 3H), 2.38 (s, 3H).

The synthetic route of 2-Chloro-5-methoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; OssiFi Inc.; Ellies, Debra; Rey, Jean-Philippe; Kimball, F. Scott; US2014/288068; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 16793-91-2, 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. 16793-91-2, name is 2-Chlorophenethyl Bromide, This compound has unique chemical properties. The synthetic route is as follows.

Compound 28. 1 -(2-chlorophenethyl)-4-(2-methoxyphenethyl)piperidine A 250 mL round bottom flask was equipped with a magnetic stir bar, and then charged with 5 grams (0.0537 mol) of 4-picoline, 8.77 grams (0.0644 mol) of 2- methoxybenzaldehyde, and 50 ml of acetic anhydride. The reaction mass was heated to reflux and maintained at that temperature for 72 hours. The reaction mixture was then cooled to room temperature, and subjected to silica chromatography. Yield of (E)-4-(2- methoxystyryl)pyridine was 7.15 grams (63%). The 7.15 grams of (E)-4-(2- methoxystyryl)pyridine was then charged into a 500 mL hydrogenation flask, to which was added 100 mL of acetic acid as well as 50 mg of Pt02. The reaction mass was subjected to 45 psi of hydrogen gas, and allowed to react at room temperature for 16 hours. The reaction mixture was then filtered through a pad of celite, evaporated, basified with aqueous Na2C03 solution, and extracted with dichloromethane. The combined extraction solvents were removed under reduced pressure via rotovap. The residue was then subjected to silica chromatography, yielding 6.1 grams (82.1 % yield) of 4-(2-methoxyphenethyl)piperidine. A 100 mL round bottom flask equipped with a magnetic stir bar was then charged with 1.0 grams of 4-(2-methoxyphenethyl)piperidine (0.0046 mol), 1 .41 grams of 2- chlorophenethyllbromide (0.0064 mol), 1.87 grams of K2C03 (0.0135 mol), and 20 mL of DMF as solvent. The reaction mass was then heated to 70 C for 24 hours. The excess DMF was removed via reduced pressure, partitioned with water and dichloromethane, the organic layer separated; excess solvent removed under reduced pressure and the residue was subjected to silica chromatography. Yield of l-(2-chlorophenethyl)-4-(2- methoxyphenethyl)piperidine was 1.12 grams (68.0% yield). 1H NMR (300 MHz, CDC13) delta 1.40-1.62 (m, 7H), 2.41-2.75 (m, 10H), 3.84 (s, 3H), 6.92-7.73 (m, 8H) ppm.

The chemical industry reduces the impact on the environment during synthesis 2-Chlorophenethyl Bromide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; UNIVERSITY OF KENTUCKY RESEARCH FOUNDATION; CROOKS, Peter, A.; DWOSKIN, Linda, P.; CULVER, John; NICKELL, Justin, R.; ZHENG, Guangrong; WO2014/144064; (2014); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 2613-34-5, A common heterocyclic compound, 2613-34-5, name is 3-Chloro-2,4-difluoroaniline, molecular formula is C6H4ClF2N, 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.

4-chloro-7-fluoro-6-nitro-quinazoline (5g, 22.0 mmol) obtained in and 3-chloro-2,4-difluoro-aniline (5.39g, 33.0 mmol) were dissolved in 2-propanol (109 mL). The mixture was heated to 80C and further stirred for 4 hours. The mixture was cooled to room temperature, diluted with acetone (100 mL), and stirred for 10 min. The resulting mixture was filtered to the title compound as a solid (7.2 lg, 92%). NMR(300 MHz, CDC13):<5 9.62(s, 1H), 8.47(s, 1H), 7.95(d, 1H), 7.53(s, 1H),7.46(s, 1H)MS(ESI+, m/z): 355 [M+H]+ The synthetic route of 2613-34-5 has been constantly updated, and we look forward to future research findings. Reference:
Patent; HANMI HOLDINGS CO., LTD.; BAE, In Hwan; BYUN, Eun Young; JU, Hae Kyoung; SONG, Ji Young; JUNG, Seung Hyun; JUN, Mi Ae; KIM, Ho Seok; JUNG, Young Hee; SHIM, Mi Yon; AHN, Young Gil; KIM, Maeng Sup; WO2012/30160; (2012); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 108-70-3, These common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, 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: An oven-dried and argon-flushed pressure tube was charged with 1,3,5-trichlorobenzene, 1,2,4-trichlorobenzene or 1,2,3-trichlorobenzene (0.25 mmol), Pd2(dba)2 (1.25 mol%), cataCXium A (5.0 mol%), boronic acid (1.5 mmol) and K3PO4 (1.5 mmol) followed by anhydrous toluene (4.0 mL). The tube was sealed with a Teflon valve and the reaction mixture was stirred at 110 C for 24 h. The cooled reaction mixture was diluted with water and extracted with DCM. The combined organic layers were dried (Na2SO4), filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography.

Statistics shows that 1,3,5-Trichlorobenzene is playing an increasingly important role. we look forward to future research findings about 108-70-3.

Reference:
Article; Reimann, Sebastian; Ehlers, Peter; Sharif, Muhammad; Spannenberg, Anke; Langer, Peter; Tetrahedron; vol. 72; 8; (2016); p. 1083 – 1094;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 96558-78-0, The chemical industry reduces the impact on the environment during synthesis 96558-78-0, name is 3-Bromo-5-chlorophenylamine, I believe this compound will play a more active role in future production and life.

Preparation of starting material 3-chloro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (SM-17) This material was prepared from 3-bromo-5-chloroaniline following a similar procedure used for SM-9, step 3. The crude product was purified by flash chromatography (RediSep Cyano, Teledyne ISCO, 0-50% EtOAc in hexanes) to afford 3-chloro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (48%) as a pale orange solid: LCMS(m/z) 172.1 (MH+), tR=0.33 minute.

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

Reference:
Patent; Costales, Abran Q.; Huang, Shenlin; Jin, Jeff (Xianming); Liu, Zuosheng; Pecchi, Sabina; Poon, Daniel; Tellew, John; US2011/52578; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 831-81-2, A common heterocyclic compound, 831-81-2, name is 4-Chlorodiphenylmethane, molecular formula is C13H11Cl, 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: In around-bottom flask, diarylmethanes (1.0 mmol), NBS (889.9 mg, 5.0 mmol) andwater (0 or 5.0 mmol) were dissolved in CHCl3 (4.0 mL). After refluxingfor 3 h in the air, the reaction mixture was quenched withNa2S2O3·5H2O, cooled to roomtemperature, washed with 5mL CH2Cl2, dried with MgSO4,and filtered to get clear organic solution. The solvent was removed reducedpressure by a rotary evaporator, and the resulting residue was subjected tocolumn chromatography on silica gel using co-solvent(ethyl acetate / petroleum ether, v/v) as eluent to give the correspondingdiaryllketones.

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:
Article; He, Chao; Zhang, Xiaohui; Huang, Ruofeng; Pan, Jing; Li, Jiaqiang; Ling, Xuege; Xiong, Yan; Zhu, Xiangming; Tetrahedron Letters; vol. 55; 32; (2014); p. 4458 – 4462;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 87851-77-2, The chemical industry reduces the impact on the environment during synthesis 87851-77-2, name is O-(3-Chloroallyl)hydroxylamine, I believe this compound will play a more active role in future production and life.

d) 2-(1-((E)-3-Chloro-2-propenyloxyimino)propyl)-5-(3,7-dioxabicyclo[4.1.0]hept-6-yl)-3-hydroxycyclohex-2-enone 7.9 g (29.5 mmol) of 2-(1-oxopropyl)-5-(3,7-dioxabicyclo[4.1.0]-hept-6-yl)-3-hydroxycyclohex-2-enone in 20 ml of methanol were mixed at room temperature with 3.5 g (32.4 mmol) of O-((E)-3-chloro-2-propenyl)hydroxylamine, and the mixture was stirred for about 10 hours. Concentration under reduced pressure gave an oil in quantitative yield which could be purified by chromatography over silica gel using cyclohexane/ethyl acetate. Yield 6.6 g. 1 H NMR (CDCl3): delta=1.13 (t); 1.93 (m); 2.20-2.75 (m); 2.90 (m); 3.13 (m); 3.50 (m); 3.98 (m); 4.52 (d); 6.10 (m); 6.35 (d); 14.3 (s).

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, O-(3-Chloroallyl)hydroxylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BASF Aktiengesellschaft; US6107254; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 452-83-5, 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. 452-83-5 name is 2-Chloro-5-fluoroaniline, 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.

General procedure: NaOt-Bu (0.240 g, 2.5 mmol), Pd(OAc)2 (0.006 g, 0.025 mmol) and [HPt-Bu3][BF4] (0.010 g, 0.035 mmol) were suspended in toluene (3 ml) in a 5 ml microwave vial. The appropriate 2-chloroaniline (0.50 mmol) and aryl bromide (0.50 mmol) were then added and the vial sealed. The reaction was then heated in the microwave reactor at 160 C for 3 h, allowed to cool, and then quenched by addition of aqueous HCl (2 M, 3 ml). The organic phase was extracted with CH2Cl2 (2×20 ml), dried (MgSO4), then filtered and the solvent removed under reduced pressure. The crude product mixture was then subjected to column chromatography (SiO2).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-5-fluoroaniline, and friends who are interested can also refer to it.

Reference:
Article; Bedford, Robin B.; Bowen, John G.; Weeks, Amanda L.; Tetrahedron; vol. 69; 22; (2013); p. 4389 – 4394;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics