Month: February 2021

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. 39065-95-7, name is 4-(Chlorodifluoromethoxy)aniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H6ClF2NO

[00713] 6-Chloro-5-iodo-3-pyridinecarboxylic acid (18 g, 62.2 mmol) was suspended in toluene (125 mL). DMF (1.446 mL, 18.67 mmol) and SOCl2 (13.63 mL, 187 mmol) were added at RT. The RM was stirred at 80C for 1 h, cooled to RT then the solvent was evaporated off under reduced pressure to give a residue that was dissolved in THF (125 mL) and cooled to – 15C. DIPEA (21.74 mL, 124 mmol) was added at -15C, and the cold mixture was treated dropwise with a solution of 4-(chlorodifluoromethoxy)aniline in THF (125 mL) over 12 min. The resulting fine orange suspension was stirred for 1 h at RT. The solvent was evaporated off under reduced pressure and the residue was dissolved in TBME (500 mL),and sequentially washed with IN HC1 (2 x 150 mL), sat. aq. NaHC03 solution (2 x 150 mL) and brine (2 x 150 mL). The aq. phases were extracted with TBME (400 mL). Combined organic phases were dried over Na2S04, filtered and concentrated under reduced pressure until crystallization began (around 100 mL). n- Heptane (800 mL) was then added with stirring and the light yellow suspension was stirred at RT for 30 min. The crystalline product was filtrated , washed with n-heptane (200 mL) and dried to afford the title product as a beige solid. LC-MS (Condition 3) tR 1.25 min, 459.0/460.7/462.1

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 39065-95-7.

Reference:
Patent; NOVARTIS AG; FURET, Pascal; GROTZFELD, Robert Martin; JONES, Darryl Brynley; MANLEY, Paul; MARZINZIK, Andreas; PELLE, Xavier Francois Andre; SALEM, Bahaa; SCHOEPFER, Joseph; SPIESER, erich Alois; WO2013/171640; (2013); 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. 51572-93-1, name is O-(2,4-Dichlorobenzyl)hydroxylamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H8Cl3NO

General procedure: A mixture of 7 (2.5 mmol), alkoxyamine hydrochloride (2.8 mmol), andpyridine (10 mL) was stirred at room temperature for 16 h, concentrated to 2 mL at reducepressure, poured into water (20 mL), and then extracted with methylene chloride (3 ¡Á20 mL). The combined organic layer was washed with dilute hydrochloride acid, waterand brine successively, dried over sodium sulfate. After evaporating the solvent, the crudeproduct was purified by silica gel column chromatography (petroleum:ethyl acetate=30:1)to give a mixture of Z and E isomers of 2. Among them, 2b, 2f, and 2j were further purifiedby silica gel column chromatography (petroleum:ethyl acetate = 2000:1) to give their Zand E isomers.

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 51572-93-1.

Reference:
Article; Meng, Chen; Li, Jian-Jun; Liang, Xiao-Mei; Zhang, Jian-Jun; Wang, Dao-Quan; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 189; 10; (2014); p. 1529 – 1538;,
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. 2268-05-5, name is 2,6-Dichlorofluorobenzene, A new synthetic method of this compound is introduced below., Safety of 2,6-Dichlorofluorobenzene

To 2,2,6,6-tetramethylpiperidine (20.07 ml_, 1 18 mmol) dissolved in Tetrahydrofuran (THF) (300 ml.) at 0 0C was added nBuLi (73.9 ml_, 118 mmol) dropwise. The solution was stirred at 0 0C for 10 minutes and cooled to -78 0C. 1 ,3- dichloro-2-fluorobenzene (15 g, 91 mmol, commercially available from e.g. Sigma- Aldrich, Apollo or Alfa Aesar) dissolved in Tetrahydrofuran (THF) (30 ml.) was added dropwise and the solution was stirred at -78 0C for 1 hour. The solution was poured on to dry ice (xs) that had been previously washed with tetrahydrofuran (3 x 100 ml.) and stirred to room temperature over 3 hours. Solvents were removed in vacuo to afford a white solid. The solid was combined with solid isolated from method a) and partitioned between ethyl acetate (200 ml.) and 2N Hydrochloric acid. The aqueous solution was extracted with ethyl acetate (3 x 100 ml_); the combined extracts were washed with brine (50 ml.) and concentrated to a crude solid. The crude solid was recrystalised from cyclohexane/toluene to afford the product 19.03 g. LC/MS = 207/209 (M-H)-, retention time = 0.90 minutes (2 minute method).

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; GLAXO GROUP LIMITED; DEAN, David Kenneth; MUNOZ-MURIEDAS, Jorge; SIME, Mairi; STEADMAN, Jon Graham Anthony; THEWLIS, Rachel Elizabeth Anne; TRANI, Giancarlo; WALTER, Daryl Simon; WO2010/125102; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

39226-95-4, name is 2,3-Dichlorobenzylamine, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 2,3-Dichlorobenzylamine

General procedure: The chiral monomer (R)-2-(2,4-bis(benzyloxy)-5-chlorobenzoyl)-1, 2,3,4-tetrahydroisoquinoline-3-carboxylic acid 9 (100 mg, 0.19 mmol), EDCI (43.7 mg, 0.228 mmol), HOBt (30.8 mg, 0.228 mmol) and 2-chloro benzylamine (0.15 mL, 1.2 mmol) in DMF (3 mL) was stirred overnight at room temperature. The organic layer was washed successively with 2 M HCl and 2 M NaOH, then dried over anhydrous/Na2SO4, filtered and evaporated under vacuum to afford a yellowish powder that was used for the next step reaction without further purification. To the anhydrous CH2Cl2 (3 mL) solution of this product cooled to 0 C under N2 was added BCl3 (1.0 M in CH2Cl2, 0.57 mL, 0.56 mmol). The reaction mixture was allowed to warm to RT and stirred for 1.5 h. Sat. NaHCO3 solution (5 mL) was added and CH2Cl2 was removed under vacuum. The aqueous residue was extracted with EtOAc (4 x 10 mL) and evaporated under vacuum to produce a brown powder. The powder was purified by column chromatography over silica gel eluted with CH2Cl2-MeOH (30: 1, v/v) to give compound 10 (82.8 mg) as a white powder, yield: 91%.

The synthetic route of 39226-95-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liang, Chuanpeng; Wu, Xingkang; Li, Zhenyu; Zhu, Jing; Lu, Chunhua; Shen, Yuemao; European Journal of Medicinal Chemistry; vol. 143; (2018); p. 85 – 96;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

33863-76-2, name is 1-Bromo-3-chloro-5-fluorobenzene, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. category: chlorides-buliding-blocks

In a three-necked flask equipped with a magnetic stirrer and placed under a nitrogen atmosphere, tert-butyl (R)-2-formylpiperidine-1-carboxylate (3.7 g, 17.3 mmol) is dissolved in tetrahydrofuran (50 mL). (3-Chloro-5-fluorophenyl) bromide (0.5 M solution in THF) (41.6 mL, 20.8 mmol) is added dropwise at -70 C. The mixture is stirred at -70 C. for 5 hours and then hydrolyzed by addition of water at 0 C. The medium is diluted with EtOAc, washed with water and with saturated NaCl solution and then dried over MgSO4 and concentrated by evaporation under reduced pressure (RP). The residue is purified by chromatography on silica gel eluted with a 6/2 cyclohexane/EtOAc mixture. 1.28 g of tert-butyl (2R)-2-[(S)-(3-chloro-5-fluorophenyl)(hydroxy)methyl]piperidine-1-carboxylate are thus obtained in the form of an oil that crystallizes, and 1.27 g of tert-butyl (2R)-2-[(R)-(3-chloro-5-fluorophenyl)(hydroxy)methyl]piperidine-1-carboxylate are obtained in the form of an oil that crystallizes. tert-Butyl (2R)-2-[(S)-(3-chloro-5-fluorophenyl)(hydroxy)methyl]piperidine-1-carboxylate: (M+Na)+=366; [alpha]D20 C.=+16.4+-0.6 (MeOH) and tert-butyl (2R)-2-[(R)-(3-chloro-5-fluorophenyl)(hydroxy)methyl]piperidine-1-carboxylate: (M+Na)+=366; [alpha]D20 C.=-46.1+-0.9 (MeOH)

The synthetic route of 33863-76-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI-AVENTIS; US2010/298377; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 220227-21-4,Some common heterocyclic compound, 220227-21-4, name is 2,4,5-Trifluorobenzene-1-sulfonyl chloride, molecular formula is C6H2ClF3O2S, 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.

Intermediate 19 1,1 -dimethylethyl (2S,4R)-2-methyl-4-{[(2,4,5-trifluorophenyl)sulfonyl]amino}-1- pyrrolidinecarboxylateTo 1 ,1-dimethylethyl (2S,4R)-4-amino-2-methyl-1-pyrrolidinecarboxylate (0.075 g, 0.38 mmol) in DCM (~5 mL) was added a solution of 2,4,5-trifluorobenzenesulfonyl chloride (0.075 g, 0.38 mmol) in DCM (~5 mL) and DIPEA (0.13 mL, 0.75 mmol). The resultant mixture was stirred at room temperature overnight, evaporated and loaded onto a 5 g silica SPE cartridge, eluting sequentially with DCM and ethyl acetate. The ethyl acetate fractions were combined and evaporated to afford the title compound (0.0942 g). LC-MS: m/z, 395 (M+H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4,5-Trifluorobenzene-1-sulfonyl chloride, its application will become more common.

Reference:
Patent; GLAXO GROUP LIMITED; WO2009/26197; (2009); 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. 348-59-4, name is 2,5-Dichlorofluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H3Cl2F

(Step 1) Synthesis of 1,4-dichloro-2-fluoro-5-nitrobenzene (0422) According to (Step 1) of Example 19, 1,4-dichloro-2-fluorobenzene (1.00 g) was dissolved instead of 1-chloro-2-fluoro-4-methylbenzene in TFA (10 mL). To the solution, fuming nitric acid (5.0 mL) was added dropwise. The mixture was stirred at room temperature for 3 hours, and then, the solution was added to an aqueous sodium bicarbonate solution. The precipitated solid was collected by filtration and dried to obtain 1.30 g of the title compound as a white solid.

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 348-59-4.

Reference:
Patent; TAIHO PHARMACEUTICAL CO., LTD.; KAWAI, Yuichi; IRIE, Hiroki; SAGARA, Takeshi; MIYADERA, Kazutaka; (63 pag.)US2017/217970; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 6775-78-6, A common heterocyclic compound, 6775-78-6, name is 6-Chloroimidazo[1,2-b]pyridazine, molecular formula is C6H4ClN3, 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.

6-Chloroimidazo[l,2-b]pyridazine (4.95 g, 31.6 mmol) [purchased from Combi-Blocks] was dissolved in 60 mL concentrated sulfuric acid, cooled in an ice bath, and nitric acid (9.9 mL, 158 mmol) was added dropwise while stirring. The reaction was stirred at 0 0C for 30 minutes, then at ambient temperature for 4.5 hours to reach completion. The reaction was poured onto ice, and the resulting aqueous mixture was neutralized with 50% NaOH aqueous solution and then extracted with EtOAc (3 x 400 mL). The organic layers were combined and washed with water (2 x 400 mL) and brine (400 mL), dried (Na2SO4), filtered and concentrated to yield the product as a yellowish powder (5.7 g, 91% yield).

The synthetic route of 6775-78-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARRAY BIOPHARMA INC.; ANDREWS, Steven, W.; HAAS, Julia; JIANG, Yutong; ZHANG, Gan; WO2010/33941; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 39226-95-4 as follows. SDS of cas: 39226-95-4

General procedure: Amine (0.386 mL) was added to Triton-B and stirred for 10 min followed by the addition of CS2 (0.321 mL) dropwise. Then dimethyl acetate carboxylate was added again dropwise. The mixture was stirred for 2.5 h. TLC plate showed the formation of some new compound. The reaction was seen continuously and formation of product was monitored with TLC. After the completion, the reaction mixture was drained into distilled water and extraction was done three times using ethyl acetate (Scheme-I)

According to the analysis of related databases, 39226-95-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Srivastava, Nitin; Saxena; Asian Journal of Chemistry; vol. 31; 1; (2019); p. 176 – 180;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 102-49-8, A common heterocyclic compound, 102-49-8, name is 3,4-Dichlorobenzylamine, molecular formula is C7H7Cl2N, 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 mixture of acid 6 (0.5 g, 1 mmol), EDCI (0.21 g, 1.1 mmol), and HOBt (0.15 g, 1 mmol) in dry CH3CN (10 mL) was stirred at room temperature for 30 min and then treated with the benzyl amine 7a (0.11 mL, 1 mmol). The mixture was stirred at room temperature for an additional 24 h. Then the solution was evaporated to dryness in vacuum. The residue was dissolved in ethyl acetate (20 mL) and washed sequentially with brine (2 .x. 5 mL), 10percent aqueous sodium carbonate (2 .x. 5 mL), 10percent aqueous citric acid (2 .x. 5 mL), and water (2 .x. 5 mL). The organic layer was dried over anhydrous sodium sulfate. Concentration of the dried extract yielded an oily residue, which was crystallized (CH2Cl2/n-C6H14) to give pure 8a amide in 27percent yield.

The synthetic route of 102-49-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fallah-Tafti, Asal; Foroumadi, Alireza; Tiwari, Rakesh; Shirazi, Amir Nasrolahi; Hangauer, David G.; Bu, Yahao; Akbarzadeh, Tahmineh; Parang, Keykavous; Shafiee, Abbas; European Journal of Medicinal Chemistry; vol. 46; 10; (2011); p. 4853 – 4858;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics