Chlorides-buliding-blocks

Reference of 623-12-1,Some common heterocyclic compound, 623-12-1, name is 1-Chloro-4-methoxybenzene, molecular formula is C7H7ClO, 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.

The appropriate quantity of stock solution C was added to a 4 mL vial containing the aryl chloride (1.00 mmol) and potasium terf-butoxide (123 mg, 1.10 mmol) in 1.5 mL of toluene. The aromatic thiol (1.00 mmol) was then added, and the vial sealed with a cap containing a PTFE septum. The mixture was heated at 110 0C until the chloroarene was consumed, as determined by GC. Silica gel (0.5 g) was then added, and solvents were evaporated under reduced pressure. The crude residue was purified by column chromatography on silica gel using hexane or a mixture of hexane and ethyl acetate as eluent. Aryl sulfides were isolated in the yields reported in Table 4.4-Methoxyphenyl phenyl sulfide (Table 4, entry 1).[49] 100 muL of stock solution C were used. A 50:1 mixture of hexane/ethyl acetate was used as chromatography eluent. 98% yield. Colorless liquid. 1H NMR (CDCl3): delta = 7.23 (d, J= 8.8 Hz5 2H), 7.06-7.02 (m, 2H), 7.00-6.93 (m, 3H), 6.71 (d, J= 8.8 Hz5 2H)5 3.62 (s, 3H). 13C NMR (CDCl3): delta = 159.7, 138.5, 135.3 (2C), 128.8 (2C), 128.1 (2C), 125.7, 124.2, 114.9 (2C)5 55.3.

The synthetic route of 623-12-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; YALE UNIVERSITY; WO2007/64869; (2007); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 4535-90-4, name is 2-Chloro-N-methylethanamine 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 4535-90-4, category: chlorides-buliding-blocks

A mixture of iraw5,-8-chloro-l-[4-(3-fluoro-pyridin-2-yl)-cyclohexyl]-5,6-dihydro-4H-2,3,5,10b- tetraaza-benzo[e]azulene (50.0 mg, 0.126 mmol), cesium carbonate (246 mg, 0.754 mmol) and 2-methylaminoethyl chloride hydrochloride (65.4 mg, 0.503 mmol) in acetonitrile (1.3 ml) was heated at 70 C for 20 h. After addition of further portions of cesium carbonate (246 mg, 0.754 mmol) and 2-methylaminoethyl chloride hydrochloride (65.4 mg, 0.503 mmol) the mixture was heated at 70 C for another 20 h. The reaction mixture was partitioned between 1 M aqueous sodium hydroxide solution (2 ml) and ethyl acetate (5 ml). The layers were separated. The aqueous layer was extracted with two 5-ml portions of ethyl acetate. The combined organic layers were concentrated in vacuo. Preparative RP-HPLC with water (0.05% formic acid) / methanol as eluent gave the title compound as formate salt. The salt was partitioned between ethyl acetate (15 ml) and 1 M aqueous sodium hydroxide solution (10 ml). The layers were separated. The aqueous layer was extracted with two 15 ml-portions of ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound (14 mg, 25%) as off-white solid. MS m/e: 455 ([M+H]+)

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-N-methylethanamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; DOLENTE, Cosimo; SCHNIDER, Patrick; WO2011/131596; (2011); 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. 104-77-8, name is 3-Chloro-N,N-diethylpropan-1-amine, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 104-77-8

a Phenylmethyl 1-[3-(diethylamino)propyl]-1H-indole-3-acetate At a temperature of about +50 C., 6.2 g (44.9 mMol) of potassium carbonate were added to a solution of 4.0 g (15.1 mMol) of phenylmethyl 1H-indole-3-acetate in 40 ml of dimethylformamide and then at the same temperature a solution of 3.0 g (20.0 mMol) of 3-(diethylamino)propylchloride in 5 ml of dimethylformamid were added dropwise. The mixture was stirred for a further hour at 50 C. and overnight at ambient temperature, heated up to 100 C. again and once more 1.0 g of 3-(diethylamino)propylchloride were added. After stirring for 5 hours at ambient temperature, the mixture was stirred into 300 ml of ice water and extracted exhaustively with diisopropylether. The combined organic extracts were washed with saturated saline solution, dried over magnesium sulphate, clarified with activated charcoal and evaporated down under reduced pressure. A colourless oil was obtained in a yield of 5.37 g (94% of theory) and was used in the following step without further purification. MS: M+ =378

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 104-77-8.

Reference:
Patent; Karl Thomae GmbH; US6114390; (2000); 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. 697-86-9, name is 2-Bromo-4,6-dichloroaniline, A new synthetic method of this compound is introduced below., Quality Control of 2-Bromo-4,6-dichloroaniline

To a toluene solution (8 mL) of 2-bromo-4,6-dichloroaniline (1 g) (CAS registry number: 697-86-9), 4-fluorophenyl acetyl chloride (788 mg) was added, followed by stirring at 90 C. overnight. The reaction mixture was cooled to room temperature, and precipitate was filtered. The precipitate was washed with toluene and then dried under reduced pressure at 50 C. to obtain the title compound (1.28 g) having the following physical property values. TLC: Rf 0.43 (hexane:ethyl acetate=1:1); 1H-NMR (CD3OD): delta 3.72, 7.02-7.08, 7.38-7.43, 7.58, 7.69.

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; Ono Pharmaceutical Co., Ltd; YASHIRO, Kentaro; WAKAMATSU, Daisuke; SAITO, Tetsuji; (53 pag.)US2017/217888; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 33406-96-1, The chemical industry reduces the impact on the environment during synthesis 33406-96-1, name is 1-Chloro-4-fluoro-2-methylbenzene, I believe this compound will play a more active role in future production and life.

General procedure: Example 3Tandem Borylation/Dehalogenation of 1-Chloro-4-fluoro-3-Substituted- and 1-Bromo-4-fluoro-3-Substituted BenzenesTandem borylation/dehalogenation was also investigated as a strategy for the ortho-borylation of arenes that are substituted with an electron-withdrawing group. The scheme below illustrates the tandem borylation/dehalogenation methodology which was investigated. As discussed above, in the case of arenes that are substituted with an electron-withdrawing group, iridium-catalyzed C-H activation-borylation of the arene is typically governed by steric effects. In tandem borylation/dehalogenation, the substrate can include an electron-withdrawing group and a sacrificial atom (e.g., a halogen such as Cl or Br) positioned para to the electron-withdrawing group, so as to sterically hinder attack of the iridium catalyst at the otherwise sterically favored position meta to the electron-withdrawing group. As a result, iridium-catalyzed C-H activation-borylation of the arene exclusively generates the ortho-borylated (electronic) product. Subsequent dehalogenation can afford exclusively the desired electronic product.[0337] General Procedure for Borylation [0338] In a nitrogen atmosphere glovebox B2Pin2 (140 mg, 0.55 mmol) was weighed into a 20 mL vial containing a magnetic stir bar. [Ir(OMe)cod]2 (6.6 mg, 0.02 mmol) and 4,4?-di-tert-butyl-2,2?-dipyridyl ligand (5.4 mg, 0.02 mmol) were weighed into two separate test tubes, each being diluted with THF (2 mL). The [Ir(OMe)cod]2 solution was transferred into the 20 mL vial containing B2Pin2. This mixture was stirred until a golden yellow clear solution was obtained. The solution containing ligand was transferred into the vial, and the mixture was stirred until it became a dark brown color solution. The substrate (1 mmol) was added to the vial, which was then sealed. The reaction mixture stirred for 24 h at rt, after which the vial was removed from the glovebox. The reaction mixture was passed through a short plug of silica eluting with a 10:1 hexane/EtOAc solution (2¡Á10 mL). The volatiles were removed by rotary evaporation affording the product, which was characterized using standard methodologies. 1-Chloro-4-fluoro-2-methylbenzene was borylated using the general procedure described above. After workup, a white solid was obtained (2.38 g, 88%): mp 48-49 C.; 1H NMR (500 MHz, CDCl3) delta 7.66 (d, J=5.5 Hz, 1H), 6.91 (d, J=9.5 Hz, 1H), 2.35 (s, 3H), 1.34 (s, 12H); 13C NMR (125 MHz, CDCl3) delta 165.4 (d, J=249.4 Hz), 141.7 (d, J=9.5 Hz), 136.5 (d, J=8.5 Hz), 129.1 (d, J=2.9 Hz), 117.7 (d, J=25.6 Hz), 84.1, 24.7, 20.4 (d, J=1.9 Hz); 19F NMR (470 MHz, CDCl3) delta 106.5; 11B NMR (160 MHz, CDCl3) delta 29.8 (br 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, 1-Chloro-4-fluoro-2-methylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Smith, III, Milton R.; Maleczka, JR., Robert E.; Li, Hao; Jayasundara, Chathurika; Oppenheimer, Jossian; Sabasovs, Dmitrijs; US2015/65743; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 445-13-6,Some common heterocyclic compound, 445-13-6, name is 3-Chloro-4-(trifluoromethyl)aniline, molecular formula is C7H5ClF3N, 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 solution of triphosgene (609 mg, 2.14 mmol) in toluene (5 mL) was added a solution of 3-chloro-4-(trifluoromethyl)aniline (100 mg, 0.51 mmol) and the mixture was refluxed at 80 C. for 0.5 h. After cooling to RT, the mixture was concentrated under vacuum and dissolved in THF (4 mL), then 3-(1-(aminomethyl)-4-oxo-4H-thieno[3,4-c]pyrrol-5(6H)-yl)piperidine-2,6-dione 2,2,2-trifluoroacetic acid (51.5 mg, 0.18 mmol) was added, followed by TEA (36 mg, 0.36 mmol). The solution was stirred at RT for 2 h then concentrated under vacuum and purified by prep-HPLC to give 1-(3-chloro-4-(trifluoromethyl)phenyl)-3-((5-(2,6-dioxopiperidin-3-yl)-4-oxo-5,6-dihydro-4H-thieno[3,4-c]pyrrol-1-yl)methyl)urea (18.6 mg, yield: 20.7%) as a white solid. MS (ESI) m/z 500.7, 502.6 [M+H]+. 1H NMR (400 MHz, DMSO-d6) delta 10.98 (s, 1H), 9.35 (s, 1H), 7.87 (s, 1H), 7.69 (d, J=9.2 Hz, 1H), 7.43 (dd, J=7.2, 8.4 Hz, 1H), 7.11 (t, J=6.0 Hz, 1H), 5.01 (dd, J=8.0, 13.2 Hz, 1H), 4.40 (d, J=6.0 Hz, 2H), 4.28 (q, J=41.6 Hz, 2H), 2.93-2.84 (m, 1H), 2.73-2.60 (m, 1H), 2.37-2.26 (m, 1H), 2.07-1.97 (m, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Chloro-4-(trifluoromethyl)aniline, its application will become more common.

Reference:
Patent; BioTheryX, Inc.; Chan, Kyle W.H.; Erdman, Paul E.; Fung, Leah; Mercurio, Frank; Sullivan, Robert; Torres, Eduardo; (112 pag.)US2018/170948; (2018); 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. 39191-07-6, name is 1-(3-Chlorophenyl)-N-methylmethanamine, A new synthetic method of this compound is introduced below., name: 1-(3-Chlorophenyl)-N-methylmethanamine

To a stirred solution of [1 -(3 -fluorobenzylsulfonyl)-2-methylindolizin-3-yl] acetic acid (Intermediate 26, 70 mg, 0.194 mmol) in DMF (2 mL) were added EDCI (46 mg, 0.23 mmol), HOBt (32 mg, 0.23 mmol) and DIPEA (0.82 mL, 0.46 mmol). The resulting solution was stirred for 5 min prior to the addition of N-methylbenzyl amine (36 mg, 0.23 mmol) and stirred overnight. The reaction was quenched with water (50 mL) and extracted with EtOAc (2 x 30 mL). The combined organic extracts were washed with water (10 mL), saturated brine (10 mL), dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by FCC eluting with 40 % EtOAc / hexane to afford the title compound (45 mg, 47 %). HPLC-MS, MH+ requires m/z=499; Found m/z=499, Rt 3.92 min (100%). 1H NMR (300 MHz, CDC13), mixture of rotamers, delta 8.13-8.03 (2d, IH), 7.82- 7.73 (2d, IH), 7.28 – 6.89 (m, 7H), 6.80 -6.75 (m, 3H), 4.57 – 4.55 (2s, 2H), 4.28-4.20 (2s, 2H), 3.93 – 3.87 (2s, 2H), 3.00- 2.97 (2s, 3H) and 2.09-1.98 (2s, 3H).

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; EVOTEC AG; BENTLEY, Jonathan, Mark; DAVENPORT, Tara; HALLETT, David, James; WO2011/138266; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 14862-52-3, name is 3,5-Dibromochlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: chlorides-buliding-blocks

Compound (M-3) (270 g, 1.0 mol, 1.0 eq) was added to a 5 L four-necked round bottom flask under nitrogen protection.Compound (N-12) (238g, 1.0mol, 1.0eq) and 2500mL of toluene, then add sodium carbonate (212g, 2.0mol, 2.0eq) and purified water (360g, 20mol, 20eq), nitrogen purge for 30mins, then Tetrakis (triphenylphosphine) palladium (11.5g, 0.01mol, 0.01eq), heated to 110 C for 15h,The reaction was monitored by HPLC for completion. Filtered with diatomaceous earth, washed the organic phase with 2000 mL of saturated brine, and dried over anhydrous sodium sulfate. Distilled to 400 mL under reduced pressure, and 2000 mL of ethanol was added dropwise to precipitate most of the solid, filtered,Drying under vacuum gave 257 g of the target compound (D-12) as an off-white solid.Yield: 67%.

The synthetic route of 14862-52-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ningbo Lumilan New Materials Co., Ltd.; Ningbo Dinghao Optoelectric Materials Technology Co., Ltd.; Zhang Yuxiang; Zhang Qingyun; Ding Huanda; Chen Zhikuan; (41 pag.)CN110551154; (2019); A;,
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. 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 4090-55-5

The flask accommodating the post-reaction solution containing intermediate 4 was filled with 121.4 g (1.2 mol) of triethylamine and 1.85 g (0.015 mol) of 4-(dimethylamino) pyridine. While the mixed solution was stirred, a mixed solution of 164.2 g (0.89 mol) of material 1 and 450 g of toluene was added thereto at 20C over 2 hours. After that, the substances were reacted at the same temperature (20C) for 8 hours. The obtained post-reaction solution was neutralized at room temperature using an aqueous solution of hydrochloric acid in an amount corresponding to the excess amount of triethylamine. The resultant solution was kept still so as to be separated into different layers. Then, the organic layer was neutralized using an aqueous solution of sodium hydrogen carbonate. The organic layer was then washed with water twice. The obtained organic layer was dried by anhydrous magnesium sulfate. The solvent and water were removed by distillation, thereby obtaining 311.2 g of phosphorus compound (3). Phosphorus compound (3) had a purity measured by GPC (gel permeation chromatography) of 95.1% by area. The yield was 94.0%.

According to the analysis of related databases, 4090-55-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DAIHACHI CHEMICAL INDUSTRY CO., LTD.; EP1632497; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 14862-52-3, The chemical industry reduces the impact on the environment during synthesis 14862-52-3, name is 3,5-Dibromochlorobenzene, I believe this compound will play a more active role in future production and life.

(3-cyanophenyl)boronic acid (25.0 g, 0.17 mol) and 1,3-dibromo-5-chlorobenzene (23.0 g, 0.08 mol),(triphenylphosphine)palladium (3.94 g, 0.34 mmol) was added thereto, followed by heating and stirring for 13 hours. The temperature was lowered to room temperature, the water layer was separated and removed, dried over anhydrous magnesium sulfate, concentrated under reduced pressure, recrystallized using chloroform and ethanol, and dried to prepare an intermediate f (44.7 g, 83% yield, MS:[M+H]+=315).

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, 3,5-Dibromochlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; LG Chem, Ltd.; Lee Jeong-ha; Cho Seong-mi; Jeong Min-u; Lee Dong-hun; Park Tae-yun; Moon Jeong-uk; Chae Mi-yeong; (39 pag.)KR2018/32519; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics