Month: February 2021

Adding a certain compound to certain chemical reactions, such as: 220227-21-4, name is 2,4,5-Trifluorobenzene-1-sulfonyl chloride, 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 220227-21-4, category: chlorides-buliding-blocks

[00373] Step A: To a solution of sodium sulfite (153 g, 1214 mmol) in water (1000 mL) was added a solution of 2,4,5-trifluorobenzene-l-sulfonyl chloride (40 g, 173 mmol) in dioxane (300 mL) dropwise. After the complete addition of sulfonyl chloride, the reaction was basified to about pH 14 by the addition of 1 N NaOH, and the reaction mixture was stirred overnight. The reaction mixture was cooled on an ice bath and acidified using 100 mL concentrated H2SO4 to about pH 1. The mixture was extracted with EtOAc and CH2CI2 and the combined organic layers were dried over a2S04, filtered and concentrated to afford 2,4,5-trifluorobenzenesulfinic acid (34 g, 100%).

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, 2,4,5-Trifluorobenzene-1-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ARRAY BIOPHARMA INC.; AICHER, Thomas Daniel; BENCSIK, Josef R.; BOYD, Steven Armen; CONDROSKI, Kevin Ronald; FELL, Jay Bradford; FISCHER, John P.; HINKLIN, Ronald Jay; PRATT, Scott Alan; SINGH, Ajay; TURNER, Timothy M.; WO2012/37393; (2012); A1;,
Chloride – Wikipedia,
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Application of 112-26-5, The chemical industry reduces the impact on the environment during synthesis 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane, I believe this compound will play a more active role in future production and life.

NaI (46.2 mg, 0.308 mmol), 1,2-bis(2-chloroethoxy)ethane (48 muL, 0.308 mmol) and Cs2CO3 (100 mg, 0.308 mmol) were mixed in DMF (1.0 mL) at rt. The mixture was protected from light, and heated to 100 C for 15 min, after which time, 7-hydroxy-2H-chromen-2-one (50 mg, 0.308 mmol) was added. The reaction was heated for 75 min more, then cooled to rt. The mixture was quenched with 1 N HCl, and extracted with EtOAc (3 x 4 mL). The combined organic layers were evaporated to dryness. The crude material was purified by flash column chromatography (silica gel, solvent gradient 0-50% EtOAc in heptane) to give 32% yield of intermediate chloride SI-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, 1,2-Bis(2-chloroethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ross, Audrey G.; Benton, Bret M.; Chin, Donovan; De Pascale, Gianfranco; Fuller, John; Leeds, Jennifer A.; Reck, Folkert; Richie, Daryl L.; Vo, Jason; LaMarche, Matthew J.; Bioorganic and Medicinal Chemistry Letters; vol. 25; 17; (2015); p. 3468 – 3475;,
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 1000572-93-9 as follows. SDS of cas: 1000572-93-9

A stirred mixture of 3,4-dichloro-5-fluorophenyl bromide (1.38 g, 5.66 mmol) and magnesium turnings (0.145 g, 5.94 mmol) in THF (8 mL) was heated at reflux under nitrogen for 30 minutes, then cooled to 0 C. To the reaction mixture was added a solution of 2-formyl-2-propyl-pyrrolidine-1-carboxylic acid tert-butyl ester (0.682 g, 2.38 mmol) in THF (2 mL) dropwise over 15 minutes. The cold reaction mixture was stirred for one hour, then quenched by the addition of saturated aqueous NH4Cl (20 mL) and extracted with EtOAc. The combined organic extracts were washed with brine, dried (MgSO4), filtered and concentrated in vacuo to a yellow oil (1.7 g). Purification by chromatography (silica, 0 to 20% EtOAc in hexanes) gave 2-[(3,4-dichloro-5-fluoro-phenyl)-hydroxy-methyl]-2-propyl-pyrrolidine-1-carboxylic acid tert-butyl ester (0.571 g, 1.41 mmol, 50%) as a white solid.

According to the analysis of related databases, 1000572-93-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Roche Palo Alto LLC; US2008/146607; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, 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 6579-54-0, Safety of 2,6-Dichlorobenzenesulfonyl chloride

General procedure: To a solution of amine (1 mmol) in 3 mL of pyridine at 0C was slowly added the appropriate benzenesulfonyl chloride (1.1 mmol, 1.1 equiv). The mixture was stirred for 12 h at 25C. The mixture was quenched with 2N HCl, extracted with EtOAc, dried over anhydrous MgSO4, and concentrated in vacuum. The crude product was purified by recrystallization and/or chromatography as noted below.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Kril, Liliia M.; Vilchez, Valery; Jiang, Jieyun; Turcios, Lilia; Chen, Changguo; Sviripa, Vitaliy M.; Zhang, Wen; Liu, Chunming; Spear, Brett; Watt, David S.; Gedaly, Roberto; Bioorganic and Medicinal Chemistry Letters; vol. 25; 18; (2015); p. 3897 – 3899;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 78068-85-6, These common heterocyclic compound, 78068-85-6, name is 3-Chloro-4-fluorobenzotrifluoride, 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.

To a stirred solution of 6-hydroxyindan-1-one (1.48 g, 10 mmol) in 30 ml of DMF was added 3-chloro-4-fluorobenzotrifluoride (2.46 g, 12 mmol) and cesium carbonate (8.40 g, 25 mmol). The reaction mixture was heated at 80 C. for 12 h. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate, washed with water (2*) and brine, dried over sodium sulfate, filtered and concentrated. The crude product was purified by silica gel chromatography, eluding with ethyl acetate (2-40%) in hexane. The final productproduct was collected as brownish yellow oil.

The synthetic route of 78068-85-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ge, Min; He, Jiafang; Lau, Fiona Wai Yu; Liang, Gui-Bai; Lin, Songnian; Liu, Weiguo; Walsh, Shawn P.; Yang, Lihu; US2007/265332; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 6276-54-6, These common heterocyclic compound, 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, 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.

3-chloropropylamine-HCL (5 g, 38.46 mmole, 1.0 equiv) was dissolved in 20 mL dry DCM under inert atmosphere. DIPEA (5.47g , 42.31 mmole, 1.1 equiv) was added via syringe at room temperature to the stirring mixture. When the solution was clear and all reagents solubilized, the reaction mixture was cooled to 00C. Under inert atmosphere, boc-anhydride (8.4 g, 38.49 mmole, 1.1 equiv) was dissolved in 5 mL dry DCM. This solution was added slowly to the stirring solution of 3-chloropropylamine-HCL at 00C. After addition, the solution was allowed to warm up to R.T. and mix for 5 hrs while monitoring for completion by TLC and LC/MS. Upon completion, 25 mL of H2O was added to the reaction at ambient atmosphere while mixing. The mixture was then diluted, transferred to a seperatory funnel, and the water layer extracted into DCM (3 x 20 mL). The organic layer was dried over Na2SO4, filtered, and evaporated to dryness to afford a crude powder. The product was purified by Hex: EtOAc silica chromatography using a CombiFlash purification system. Product eluted at 2 : 1 Hex: EtOAc and collected fractions were evaporated to dryness to afford S1-1 as a white powder (MW: 193.67 g/mol, 6.08 g, 82% yield).1H NMR (400 MHz, CDCl3): 3.58 (t, J = 6.4 Hz, 2H), 3.27 (m, 2H), 1.96 (m, 2H), 1.43 (s, 9H).

Statistics shows that 3-Chloropropan-1-amine hydrochloride is playing an increasingly important role. we look forward to future research findings about 6276-54-6.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; SHOKAT, Kevan, M.; GENTILE, Daniel; MOSS, Steven; (380 pag.)WO2018/112420; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 309721-44-6, name is 2-Bromo-1-chloro-3-fluorobenzene, 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 309721-44-6, Quality Control of 2-Bromo-1-chloro-3-fluorobenzene

To a solution of 2-bromo-l-chloro-3-fluorobenzene (6.0 g, 29 mmol) in tetrahydrofuran (30 mL) at -70 C was added dropwise lithium diisopropylamide (2 M in tetrahydrofuran/n-heptane, 22 mL, 43 mmol). The resulting solution was stirred at -70 C for 0.5 hour. Then N, N – dimethylformamide (4.2 g, 57 mmol) was added slowly, and stirring was continued at -70 C for another 0.5 hour. On completion of the reaction by TLC [petroleum ether: ethyl acetate = 10: 1, Rf=0.6], the reaction was quenched with saturated aqueous ammonium chloride (2 mL) at 0 C and extracted with acetate ethyl (3 chi 20 mL). The combined organic extracts were concentrated to give compound A-49 (4.0 g, 58% yield) as a yellow solid. -NMR (CD3OD, 400 MHz): delta 7.64-7.57 (m, 1H), 7.21-7.17 (m, 1H), 6.02 (s, 1H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; FORUM PHARMACEUTICALS, INC.; ACHARYA, Raksha; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; COOK, Andrew, Simon; HARRISON, Bryce, Alden; MCRINER, Andrew, J.; (127 pag.)WO2016/201096; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, 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. SDS of cas: 6579-54-0

Taking 245 mg 2,6-dichlorobenzenesulfonyl chloride dissolved into 20 ml anhydrous methanol, stirring 20 min, add m-phenylenediamine 450 mg and triethylamine 3 ml, in 70 C under stirring 12 h cooling, methanol, water, extracted with ethyl acetate three times, the combined organic phase, water washing, water-free MgSO4Drying, evaporating the solvent, purification with silica gel column chromatography, eluting agent volume ratio: AcOEt: petroleum ether=1:4, to obtain white solid N,N’-bis(2,6-dichlorobenzenesulfonyl)m-phenylenediamine 515 mg, yield 98%.

The synthetic route of 6579-54-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jishou University; Xiao Zhuping; Ni Weiwei; Fu Zijuan; Yi Juan; Zhou Tianli; (21 pag.)CN109096156; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

118-69-4, name is 2,6-Dichlorotoluene, 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. Safety of 2,6-Dichlorotoluene

5 g of catalyst, as described in examples 3 and 4, was loaded in the reactor along with the diluent corundum particles (1: 1 by weight) and the reaction was performed under the following conditions. A reaction temperature of 350 to [400C] was used, and the GHSV comprised between 650-750 [H-1.] The contact time consisted of 4.8 to 5.5 seconds. The mole ratio of 2,6-DCT : H20 : NH3: air: N2 was 1: 15: 3-4: 21, the molar concentration of 2,6- DCT was 2.4 % and the ratio of [0/NH3] was 1. [1 %.]

The synthetic route of 118-69-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TESSENDERLO CHEMIE S.A.; WO2003/101939; (2003); A2;,
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. 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Chloro-N,N-dimethylethanamine hydrochloride

A mixture of the 4-hydroxybenzaldehyde (100g, 0.82mol) and anhydrous K2CO3 (330g,2.5mol) in EtOAc (1000mL) was stirring at 80 C till the disappearance of the startingmaterials 4-hydroxybenzaldehyde. Then 2-chloro-N, N-dimethylethanaminehydrochloride (118.69g, 0.83mol) was added into the reaction system and continued tostir until the reaction finished. After reaction, the mixture was filtered and the filtratewas washed with water and dried with Na2SO4. The extraction was filtered and thefiltrate was evaporated under reduced pressure to recycle the ethyl acetate and give thecrude mass which was further evaporated under high vacuum (bp142 -144oC/0.533 kPa)to give pale yellow oil(181.42g, 94%).

According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Feng, Chengliang; Yan, Bin; Yin, Guibo; Chen, Junqing; Ji, Min; Synlett; vol. 29; 17; (2018); p. 2257 – 2264;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics