Month: June 2021

Related Products 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.

(R)-N2-Indan-1-yl-4H-benzo[d][1,3]oxazine-2,5-diamine (example 2) (150 mg, 0.54 mmol) was dissolved in 5 mL pyridine and 3,5-difluoro-benzenesulfonyl chloride (112 mg, 0.53 mmol) was added. The reaction mixture was stirred at room temperature overnight. 1N HCl was added until pH5. The mixture was extracted three times with ethyl acetate (50 mL each). The organic phases ware pooled, dried with sodium sulfate, filtered and evaporated. The crude product was purified by a silica gel column chromatography with heptane/ethyl acetate 1:1 to give a white solid (24 mg, 9%), MS: m/e=456.0 (M+H+).

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; Kolczewski, Sabine; Roche, Olivier; Steward, Lucinda; Wichmann, Juergen; Woltering, Thomas; US2010/63042; (2010); 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. 202925-07-3, name is 2-Chloro-1-fluoro-4-methoxybenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 2-Chloro-1-fluoro-4-methoxybenzene

A mixture of 3-chloro-4-fluoroanisole (2.52 g, 15.7 mmol, 1.0 eq.), silver trifluoroacetate (8.53 g,38.6 mmol, 2.5 eq.), iodine (7.94 g, 31.3 mmol, 2.0 eq.) and chloroform (100 mL) is stirred at r.t. for 16 h. The reaction mixture is filtered through a silica plug on a fritted funnel and rinsed with chloroform. The filtrate is washed successively with an aqueous solution of Na2S2O3, water and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue is purified by flash chromatography on silica gel to afford the expected product.

The synthetic route of 202925-07-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GALAPAGOS NV; LES LABORATOIRES SERVIER; LABEGUERE, Frederic, Gilbert; HENG, Rama; ALVEY, Luke, Jonathan; AMANTINI, David; BREBION, Franck, Laurent; DE CEUNINCK, Frederic, Andre; DEPREZ, Pierre, Marc, Marie, Joseph; GOSMINI, Romain, Luc, Marie; JARY, Helene; PEIXOTO, Christophe; POP-BOTEZ, Iuliana, Ecaterina; VARIN, Marie, Laurence, Claire; (147 pag.)WO2017/211667; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 83121-15-7, The chemical industry reduces the impact on the environment during synthesis 83121-15-7, name is 3,5-Dichloro-2,4-difluoroaniline, I believe this compound will play a more active role in future production and life.

Example 3 2,4-Difluoro-3,5-dichlorophenyl isocyanate Hydrogen chloride was passed into a well-stirred solution of 39.6 gm (0.20 mol) of 2,4-difluoro-3,5-dichloroaniline in 400 ml of toluene until a precipitate no longer separated out. The heterogeneous mixture thus obtained was cooled to 5 to 10 C. At this temperature, 40 gm (0.4 mol) of phosgene were passed in, with stirring. The mixture was then heated slowly, with stirring, so that after about two hours a temperature of 100 to 105 C. was reached. Stirring was then continued for seven hours at this temperature. During this time, a clear solution was formed, and hydrogen chloride was liberated. Nitrogen was then passed into the mixture for one hour at the same temperature to drive off the excess phosgene. Thereafter the solvent was distilled off, in vacuo at the end. The crude product which remained was distilled in a water pump vacuum. Yield: 35.4 gm (0.158 mol; 79% of theory), B.p.: 100-104 C./20 mbar.

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-Dichloro-2,4-difluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Celamerck GmbH & Co. KG; US4457943; (1984); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application 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.

[2-CHLORO-4-TRIFLUOROMETHYL-PYRIMIDINE-5-CARBOXYLIC] acid cyclopentylmethyl-amide [(100MG] Example 183a), 2-chloro-5-fluoroaniline (ex-Fluorochem, 237mg), and 1,4-dioxan [(1] ml) were stirred at [100C] under nitrogen for 18h. The cooled reaction mixture was evaporated in vacuo, treated with ethyl acetate (5 ml), washed with aqueous 2M hydrochloric acid (2 x [3ML),] followed by water (2×3 ml), and dried [(NA2SO4).] The solution was evaporated in vacuo and the residue purified by mass directed autopreparative purification to give the title compound (35mg). NMR 8 [(CDCL3)] 1.2-1. 35 (2H, m), 1.53-1. 76 (>4H, [M] + H20), 1.78-1. 90 (2H, m), 2.17 [(1H,] [Q),] 3.41 (2H, dd), 5.9 [(1H,] brt), 7.0-7. 11 (2H, m), 7.65-7. 7 [(1H,] m) 8.56 [(1H,] dd), 8.79 [(1H,] s). LC/MS t = 3.67 min, Molecular ion observed [MH+] 417 consistent with the molecular formula C18H17ClF4N4O

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:
Patent; GLAXO GROUP LIMITED; WO2004/18433; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 445-14-7, name is 2-Amino-4-chlorobenzotrifluoride, 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. COA of Formula: C7H5ClF3N

To a solution of 5-chloro-2-(trifluoromethyl)aniline (0.587 g, 3.0 mmol) in acetic acid (1.5 mL, 26.2 mmol) at rt was added concentrated hydrochloric acid (3.0 mL, 99 mmol) in one portion. To the resulting mixture at -10 to -5 oC was added a solution of sodium nitrite (0.248 g, 3.60 mmol) in water (0.9 mL) over 10 min. The mixture was stirred at -10 to 0 oC for 45 min before a solution of tin(II) chloride dihydrate (1.489 g, 6.60 mmol) in concentrated hydrochloric acid (3.0 mL, 99 mmol), pre-cooled at 0 oC, over 10 min. The mixture was stirred at -10 to 0 oC for 1 h and then at 0 to 5 oC for 1 h. The precipitating product, (5-chloro-2-(trifluoromethyl)phenyl)hydrazine, HCl (0.49 g, 1.983 mmol, 66.1percent yield), was collected as a pale solid by suction filtration and dried at 50 oC under vacuum. MS (ESI) m/z: 211.08 [M+H]+; 1H NMR (500 MHz, METHANOL-d4) delta 7.69 (d, J=8.3 Hz, 1H), 7.28 – 7.19 (m, 2H).

The synthetic route of 2-Amino-4-chlorobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; JALAGAM, Prasada Rao; NAIR, Satheesh Kesavan; PANDA, Manoranjan; FENG, Jianxin; WANG, Wei; LIU, Chunjian; ELLSWORTH, Bruce A.; SARABU, Ramakanth; SWIDORSKI, Jacob; HARTZ, Richard, A.; XU, Li; YOON, David S.; BENO, Brett R.; REGUEIRO-REN, Alicia; (457 pag.)WO2019/67702; (2019); 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. 1205-71-6, name is 4-Chloro-N-phenylaniline, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C12H10ClN

In a 250 ml round bottom flask, 7-bromobenzo [b] naphtho [2,1-d] furan (12 mmol), copper iodide (15 mmol), potassium tert-butoxide (65 mmol), 1,2-di Aminocyclohexane (12 mmol) and (12 mmol) (4-chloro-phenyl) -phenylamine were added to dry 1,4-dioxane (100 ml) and refluxed for 48 hours under N2 atmosphere. The intermediate was cooled to room temperature, added to water, and then filtered through a pad of celite while extracting with dichloromethane, then washed with water, and dried over anhydrous magnesium sulfate. After filtration and evaporation, the crude product was purified by silica gel column chromatography to obtain Intermediate product HT012-1.

According to the analysis of related databases, 1205-71-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Tianma Organic Shine Display Co., Ltd.; Zhang Lei; Gao Wei; Niu Jinghua; Dai Wenpeng; Xiao Wenjing; Lu Yan; Zhu Hongyan; (28 pag.)CN110746391; (2020); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 367-22-6,Some common heterocyclic compound, 367-22-6, name is 4-Chloro-3-fluoroaniline, molecular formula is C6H5ClFN, 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.

Step C(2S)(M)-[7-[(4-c loro-3-fluorop enyl)amino]-4-(8-fluoro-5-m2-methyl-1 -oxo-1 ,2-dihyd -3-isoquinolinyl][( 1, 1-dimethylethyl)oxy]ethanoic acid[00186] A degassed mixture of (S)(M)-me y 2-(7-bromo-4-(8-fluoro-5-methylchroman-6- yl)-2-methyl-1-oxo-1 ,2-dihydroisoquinolin-3-yl)-2-(tert-butoxy)acetate (22.00 mg, 0.040 mmol), 4-chloro-3-fluoroaniline (1 1.72 mg, 0.081 mmol) and sodium tert-butoxide (1 1 .61 mg, 0.121 mmol) in 1 ,4-Dioxane (1.0 mL) was treated with Pd2(dba)3 (2.084 mg, 2.013 muetaetaomicronIota) and 2- dicyclohexylphosphino-2′-(N,N-dimethyl-amino)biphenyl (3.17 mg, 8.05 mumol) and then irradiated in the microwave at 100 C for 10 minutes. The mixture was diluted with ethyl acetate and washed with saturated sodium bicarbonate, followed by brine. The organic phase was dried over sodium sulfate, filtered and concentrated. The crude residue in methanol (1 .0 mL), tetrahydrofuran (THF) (1 .0 mL) and water (0.2 mL) was treated with lithium hydroxide (19.28 mg, 0.805 mmol) and then heated at 65 C for 4 hours. The mixture was concentrated, water was added and the mixture was adjusted to pH 3 with 1 N hydrochloric acid. The mixture was extracted with ethyl acetate and the extracts were washed with brine, dried over sodium sulfate, filtered and concentrated. The residue was purified by reverse phase chromatography to afford the title compound as a tan solid (1 1.8 mg, 49%). 1H NMR (400MHz ,CHLOROFORM-d) delta = 8.10 (m, 1 H), 7.32 – 7.17 (m, 2 H), 6.93 (m, 1 H), 6.89 – 6.74 (m, 3 H), 5.18 (s, 1 H), 4.31 (m, 2 H), 3.71 (s, 3 H), 2.78 – 2.67 (m, 2 H), 2.15 (m, 2 H), 1 .96 (s, 3 H), 1.23 (s, 9 H); LC/MS (m/z) ES+ = 598 (M+1 ).

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

Reference:
Patent; GLAXOSMITHKLINE LLC; DE LA ROSA, Martha Alicia; HAYDAR, Simon, N.; JOHNS, Brian Alvin; VELTHUISEN, Emile Johann; WO2012/102985; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane, 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 112-26-5, category: chlorides-buliding-blocks

7.7Ig (50 mmo 1) of 2,6-dimethoxyphenol and 8.42 g (45 mmol) of 1,2- (dichloroethane) ethane were added to IOOml of acetonitrile at a temperature of 20 C with stirring , 6.06 g (108 mmol) of potassium hydroxide was added thereto, and the temperature was raised to 82 C. After 92 hours of reaction, acetonitrile was distilled off at atmospheric pressure to obtain orange turbid liquid.[0027] IOOml dichloromethane was added to the above-mentioned orange turbid liquid 1, the insoluble matter was filtered off, washed twice with 50 ml of IM sodium hydroxide solution and twice with saturated sodium chloride solution (20 C) Dried over anhydrous magnesium sulfate and evaporated to dryness at atmospheric pressure to give a yellow oily liquid 2;[0028] To the above yellow oily liquid 3 was added 25 ml of diethyl ether, the temperature was raised to 35 C, the insoluble matter was filtered off, cooled to _15 C, cooled for 3 hours, the liquid was stratified, and the pale yellow solution was taken and cooled to -15 C (2- (2,6-dimethoxyphenoxy) ethoxy) ethane in a yield of 69.33% and a purity of 98.42% as a white powder

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, 1,2-Bis(2-chloroethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Xi’an Modern Chemical Institute; Lu Tingting; Ji Yueping; Zhang Lijie; Liu Yajing; Wang Wei; Pan Yongfei; Xu Minghui; Mo Hongchang; Lu Xianming; Ding Feng; (6 pag.)CN106946664; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 60811-21-4, 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. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a dry-ice/ethanol cooled solution of compound S1 (20.0 g, 0.95 mol) in THF (200 mL) was added 2 M LDA (52 mL, 1.05 mol) dropwise over 30 min. After addition, the reaction mixture was stirred at this temperature for 30 min followed by the addition of DMF (10.5 g, 1.43 mol). The reaction was stirred for 30 min and warmed to room temperature slowly. The reaction mixture was then quenched with aq. NH4Cl (100 mL) and extracted with ethyl acetate (500 mL). The organic phase was washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated. The residue was purified by column chromatography on silica gel (eluted with petroleum ether/ethyl acetate=1:0 to 50:1) to give compound S2 (10 g, yield 40%) as a yellow oil.

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, 4-Bromo-2-chloro-1-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WILES, Jason, Allan; PHADKE, Avinash, S.; DESHPANDE, Milind; AGARWAK, Atul; CHEN, Dawei; GADHACHANDA, Venkat, Rao; HASHIMOTO, Akihiro; PAIS, Godwin; WANG, Qiuping; WANG, Xiangzhu; (905 pag.)WO2017/35353; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 883499-24-9, name is 1-Bromo-2-chloro-3-fluorobenzene, 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. Application In Synthesis of 1-Bromo-2-chloro-3-fluorobenzene

In a nitrogen atmosphere, a flask containing 1-bromo-2-chloro-3-fluorobenzene (10.2 g, 49 mmol, 1 eq.), 1OH3NP14(m) (23.8 g, 1 eq.), potassium carbonate (13.4 g, 2 eq.), and NMP (70 ml) was heated and stirred at 180 C. After completion of the reaction, the reaction liquid was cooled to room temperature, and NMP was distilled off under reduced pressure. Subsequently, water and toluene were added thereto, and the mixture was partitioned. Subsequently, purification was performed by silica gel column chromatography to obtain ?1Br2CL3Px (3NP14(m))?

The synthetic route of 1-Bromo-2-chloro-3-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kwansei Gakuin Educational Foundation; JNC Corporation; HATAKEYAMA, Takuji; KONDO, Yasuhiro; NAKAMOTO, Keiichi; YANAI, Motoki; (190 pag.)US2018/94000; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics