Tag: M.W=200-300

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. 121-27-7, name is 5-Chloro-2-(4-chlorophenoxy)aniline, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C12H9Cl2NO

In the reactor was added 800kg 44.45% nitrosyl sulfuric acid solution,Warmed to 25 C,The melted 700kg amino material slowly added to the reactor,The reaction was incubated at 30 ~ 35 2 hours to complete the reaction of the amino compound,

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 121-27-7.

Reference:
Patent; Jiangsu Yi Ke Chemical Co., Ltd.; Yi Jianghua; Xie Shoulei; Yu Qianli; (6 pag.)CN107353185; (2017); 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. 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 61881-19-4

Compound 4 (0.91 g, 4.09 mmol) was dissolved in 5ml acetone, and then2,2,2-trifluoro-N-phenylethanimidoyl chloride (0.87 g, 4.19 mmol) and potassiumcarbonate (0.58 g, 4.19 mmol) were successively added. After stirring at roomtemperature for about 18 h, the mixture was evaporated under reduced pressure.The residue was purified by column chromatography on silica gel (200-300 mesh) toafford pure 8, yield 87%. TLC (ethyl acetate/petroleum ether 4:1, V:V); 1H NMR (400MHz, CDCl3) delta: 1.31 (m, 3H, CH3), 1.35 (m, 3H, CH3), 3.15 (m, 1H, CH), 3.22 (m, 1H,CH), 3.50 (s, 3H, CH3), 3.59 (s, 3H, CH3), 3.61 (m, 2H, CH2), 3.69 (m, 1H, CH), 3.75(m, 1H, CH), 5.25 (s, 1H, CH); 6.88(m, 1H, CH), 7.14 (s, 1H, CH), 7.33 (m, 1H, CH),7.44 (s, 1H, CH); 7.59 (s, 1H, CH) ; 13C NMR (100 MHz, CDCl3) delta: 15.6, 17.8, 59.2,61.1, 67.8, 70.7, 79.7, 82.0, 96.2, 117.3, 119.5, 120.4, 125.4, 129.2, 129.4,133.9, 143.6; MS (ESI) cal for C18H24F3NO5 [M+Na]+ 414.14988, found [M+Na]+414.15034.

According to the analysis of related databases, 61881-19-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Kai; Liu, Shenglan; Liu, Anjun; Chai, Hongxin; Li, Jiarong; Lamusi; Beilstein Journal of Organic Chemistry; vol. 13; (2017); p. 2603 – 2609;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 468075-00-5, name is 2-Bromo-1-chloro-4-(trifluoromethoxy)benzene, 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. Safety of 2-Bromo-1-chloro-4-(trifluoromethoxy)benzene

Into a two-dram vial was added-2-bromo-1-chloro-4-(trifluoromethoxy)benzene (100 mg, 0.363 mmol), the title compounds from Example 3 Step B (100 mg), and SPhos biaryi precatalysis (26.2 mg, 0.036 mmol), cesium carbonate (237 mg. 0.726 mmol) followed by 1,4-dioxane (2 ml). The mixture was degassed by N2 for 5 mm, then heated at 100C for 24 h. Concentrate to remove solvents. The afforded crude was purified with normal phase silica gel chromatography (0 to 100% EtOAc in 1:1 mixed hexanes/DCM) to give desired product (as a mixture of 2).

The synthetic route of 2-Bromo-1-chloro-4-(trifluoromethoxy)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; CHELLIAH, Mariappan; CHU, Hong Dong; COX, Jason, M.; DEBENHAM, John, S; EAGEN, Keith; LAN, Ping; LONDON, Clare; PLOTKIN, Michael, A.; SHAH, Unmesh; SINZ, Christopher Joseph; SUN, Zhongxiang; VACCARO, Henry, M.; VENKATRAMAN, Skikanth; WO2014/59232; (2014); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 18282-59-2, name is 4-Bromo-1,2-dichlorobenzene, 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. Formula: C6H3BrCl2

Mg (1.93 g, 79.4 mmol) was suspended in Et2O (50 ml). A chip of I2 was added, then heated to 45° C. 3,4-dichlorobenzylchloride (5.50 ml, 39.7 mmol) in Et2O (50 ml) was added slowly and the mixture was stirred at 45° C. for 2 h, then cooled to 23° C. In a second flask, CuCN (71 mg, 0.79 mmol) was suspended in Et2O (20 ml), then cooled to -30° C. under N2. The Grignard reagent was cannulated into the second flask, then warmed to -15° C. Compound 70 (4.75 g, 7.94 mmol) in Et2O (50 mL) was added dropwise. The mixture was stirred at -15° C. overnight, then warmed to 23° C. and stirred for 24 h. The reaction was quenched with 25percent aqueous sodium citrate at 0° C. and the product extracted with EtOAc. The combined organic extracts were washed with brine, dried (Na2SO4), filtered, and concentrated. Purification by silica gel chromatography (eluant: 3percent to 6percent EtOAc:hexane) gave 3.73 g (4.9 mmol, 62percent) of the product 71. MS (M+1): 759.

The synthetic route of 4-Bromo-1,2-dichlorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SCHERING CORPORATION; US2005/182095; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 13918-92-8, 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 13918-92-8 as follows.

Intermediate 14Preparation of N- [5 -bromo-2-(methyloxy)- 3 -pyridinyll -2,4-difluorobenzenesulfonamideTo a cooled (0 0C) solution of 5-bromo-2-(methyloxy)-3-pyridinamine (20.3 g, 100 mmol) in Pyridine (200 rnL) was added slowly 2,4-difluorobenzenesulfonyl chloride (21.3 g, 100 mmol) over 15 min (reaction became heterogeneous). The ice bath was removed and the reaction was stirred at ambient temperature for 16 h, at which time the reaction was diluted with water (500 mL) and the solids filtered off and washed with copious amounts of water. The precipitate was dried in a vacuum oven at 50 0C to give N-[5-bromo-2- (methyloxy)-3-pyridinyl]-2,4-difluorobenzenesulfonamide (12 g, 31.6 mmol, 31.7 % yield). MS (ES) m/e 380.9, 379.0 (M + H)+.

According to the analysis of related databases, 13918-92-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2008/157191; (2008); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 61881-19-4, These common heterocyclic compound, 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, 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 a typical experimental procedure, a dry, two-necked, 50 mL round-bottomed flask equipped with a nitrogen inlet was charged with 5 mL of dry MeCN, 0.117 g (1.0 mmol) of indole and 0.24 g (1.0 mmol) of NaH. The solution was stirred under a nitrogen atmosphere at room temperature for 30 min, then a solution of 2a (1.0 mmol in 2 mL of dry MeCN) was added dropwise via a syringe. The mixture was stirred at room temperature for 20 h under an N2 atmosphere and then filtered. After removing the solvent under reduced pressure, the crude product was purified by preparative thin-layer chromatography on silica gel [eluent: n-hexane/EtOAC, 4:1] to give the product 4a. The products obtained from indole-3-carbaldehyde were purified by recrystallization from EtOH (twice).

Statistics shows that 2,2,2-Trifluoro-N-phenylacetimidoyl chloride is playing an increasingly important role. we look forward to future research findings about 61881-19-4.

Reference:
Article; Darehkordi, Ali; Rahmani, Fariba; Hashemi, Vahide; Tetrahedron Letters; vol. 54; 35; (2013); p. 4689 – 4692;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 328-72-3, 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. 328-72-3 name is 3,5-Bis(trifluoromethyl)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.

STR7 Preparation of 3,5-bis-(trifluoromethyl)-benzonitrile By the method of Example 3, 124 g of 1-chloro-3,5-bis-(trifluoromethyl)-benzene in 120 ml of ethyl methyl ketone gave 61.4 g (51.2% of theory) of 3,5-bis-(trifluoromethyl)-benzonitrile (b.p.45 mbar: 88 C.). After 20 hours, the conversion was approximately 60%. 4.5% of coupling products had formed.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Bis(trifluoromethyl)chlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Bayer Aktiengesellschaft; US6162942; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 38762-41-3, The chemical industry reduces the impact on the environment during synthesis 38762-41-3, name is 4-Bromo-2-chloroaniline, I believe this compound will play a more active role in future production and life.

Description 13; (4-Bromo-2-chlorophenyl)-(tetrahydropyran-4-yl)-amine (D13); A mixture of 4-bromo-2-chloro-phenylamine (0.5 g, 2.422 mmol), tetrahydropyran-4- one (1.308 ml, 10.898 mmol), and sodium triacetoxyborohydride (2.31 g, 10.898 mmol) in DCE (20 ml) was stirred at room temperature for 16 h. The reaction mixture was washed with NaHCO3 (aqueous sat. solution), dried (Na2SO4) and the solvent was evaporated in vacuo. The residue was purified by column chromatography (silica gel; heptane/DCM up to 40% as eluent). The desired fractions were collected and evaporated in vacuo to yield compound D13 (0.383 g, 52%) as white solid. LCMS: MW (theor): 289; [MH+]: 290; RT (min): 4.39 (Method 1).

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-chloroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ORTHO-MCNEIL-JANSSEN PHARMACEUTICALS, INC.; ADDEX PHARMA S.A.; CID-NUNEZ, Jose, Maria; TRABANCO-SUAREZ, Andres, Avelino; MACDONALD, Gregor, James; WO2010/60589; (2010); 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. 64628-73-5, name is 3-Chloro-4-(trifluoromethoxy)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 64628-73-5

An ice-cold mixture of 98% H2SO4 (0.75 mL) and water (2.25 mL) was added to 3-chloro-4-(trifluoromethoxy)aniline (53) (1 .00 g, 4.73 mmol) and the resulting salt was crushed (using a glass rod) and cooled in an ice bath. A solution Of NaNO2 (359 mg, 5.20 mmol) in cold water (0.75 mL, then 0.25 mL) was added drop-wise, and the mixture was stirred at 0 0C for 12 min. A solution of urea (42.6 mg, 0.709 mmol) in cold water (0.25 mL) was added, and the mixture was stirred at 0 0C for 3 min. Finally, a solution of KI (1.65 g, 9.94 mmol) in cold water (1.6 mL, then 0.2 mL) was added slowly, and the mixture was stirred at room temperature for 10 min, and then at 52 C for 2 h. The resulting cooled mixture was diluted with ice-water (45 mL) and extracted with CH2Cl2 (4x 50 mL). The extracts were sequentially washed with an aqueous solution of Na2SO3 (30 mL of 0.5%) and then with water (40 mL) and finally concentrated carefully under reduced pressure at 17 C. The resulting oil was chromatographed on silica gel, eluting with pentane, to give 2-chloro-4-iodo- 1 -(trifluoromethoxy)benzene (54) (1.24 g, 81%) as a colourless oil (a white solid on freezing); 1H NMR (CDCl3) delta 7.82 (d, J = 2.1 Hz, 1 H), 7.61 (dd, J = 8.6, 2.1 Hz, 1 H), 7.05 (dq, J = 8.6, 2.0 Hz, 1 H); HRAPCIMS calcd for C7H3ClF3IO mlz (M+) 323.8834, 321.8864, found 323.8834, 321.8861.

The synthetic route of 64628-73-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLOBAL ALLIANCE FOR TB DRUG DEVELOPMENT; DENNY, William, Alexander; THOMPSON, Andrew, M.; BLASER, Adrian; MA, Zhenkun; PALMER, Brian, Desmond; SUTHERLAND, Hamish, Scott; KMENTOVA, Iveta; WO2011/14774; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1940-29-0, 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. 1940-29-0 name is 4-Bromo-3,5-dichloroaniline, 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.

(4-Bromo-3,5-dichloro-phenyl)-[5-methanesulfonyl-2-(4-methoxy-benzyl)-2H- [l,2,4]triazol-3-yl]-amine In a 25 mL round bottle, 5-chloro-l-(4-methoxybenzyl)-3-(methylsulfonyl)-lH-l,2,4-triazole (200 mg, 663 muiotaetaomicron, Eq: 1.00) was combined with DMF (3 mL) to give a colorless solution. 4- Bromo-3,5-dichloroaniline (160 mg, 663 muiotaetaomicron, Eq: 1.00) and sodium 2-methylpropan-2-olate (127 mg, 1.33 mmol, Eq: 2.00) were added. The reaction was degassed by nitrogen for 5 min. The resulting solution was heated to 85 C overnight under nitrogen. The reaction mixture was cooled and diluted with 20 mL H20, added Ether (30×2 mL) to extract the product, dried the organic layer over anhydrous Na2S04, concentrate the solution, purify the compound by column (Hexanes/EtOAc = 70/30) to afford the compound 180mg (54%). MH+ 507.0

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-3,5-dichloroaniline, and friends who are interested can also refer to it.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; DING, Qingjie; JIANG, Nan; WEIKERT, Robert James; WO2014/135472; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics