Month: September 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. 108-70-3, name is 1,3,5-Trichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C6H3Cl3

In a nitrogen-filled glove box, a 50 mL pressure flask wascharged with 1,3,5-trichlorobenzene (13.68 g, 75.40 mmol),0.67 mL of chloroform (1.00 g, 8.37 mmol), aluminum trichloride(1.22 g, 9.14 mmol), and a magnetic stir bar. This mixture washeated to 90 C for 2 h under an atmosphere of nitrogen. After thistime the mixture was allowed to cool to room temperature and 20 ml of HCl (0.1N) was added drop-wise over this mixture whichwas cooled in an ice bath. The purple suspension immediatelyturned into a yellow solution that was then extracted from theaqueous byproducts using 50 mL of chloroform in a separatoryfunnel. The organic layer was dried over magnesium sulfate for 1 hand filtered over a scintillated glass frit. The yellow solution wasimmediately concentrated under vacuum and the obtained oilymaterial was added to 40 mL of hexanes which resulted in theimmediate precipitation of a white solid. The solid was collected ona frit, and washed with hexanes until the washings were colorless.The white solid was dried under vacuum to get an 80% yield whichwas used in the next step without further purification. m.p. 246-248C. 1H NMR (400 MHz) (CDCl3): d 6.68 (s, 1H, CHPh), 7.23e7.24(d, 3H, J 2.3 Hz), 7.35e7.36 (d, 3H, J 2.3 Hz). 13C NMR(100.61 MHz): delta 49.80(CH), 128.43, 130.00, 133.78,133.82, 137.07,137.90. The synthesis has been modified slightly and the purificationprocess as well. Characterization data of this compound is inagreement with those reported in the literature [16].

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 108-70-3.

Reference:
Article; Neier, Eric; Arias Ugarte, Renzo; Rady, Nader; Venkatesan, Swaminathan; Hudnall, Todd W.; Zakhidov, Alexander; Organic electronics; vol. 44; (2017); p. 126 – 131;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 932-96-7, A common heterocyclic compound, 932-96-7, name is 4-Chloro-N-methylaniline, molecular formula is C7H8ClN, 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 air, K2HPO4 (10 mol %, 4.35mg), PMHS (242 mul), amine (0.25 mmol), formic acid (4.6equiv ,43.3mul), 18-crown-6 (20mol %, 13.2mg) 4A MS(10mg) and 2 ml THF were added into a tube equipped with a water condenser. The reaction mixturewas stirred at 80C for 12 hours. The yields of isolated products were reported. The mixture was filtered through a silica gelcolumn with petroleum ether and ethyl acetate as the eluent. The resultant solution was concentrated and purified by silica gelcolumn chromatography to give the corresponding product.

The synthetic route of 932-96-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Huang, Yan; Deng, Wei; Lin, Bo-Lin; Chinese Chemical Letters; (2019);,
Chloride – Wikipedia,
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Related Products of 2533-69-9, 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. 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of methyl 2,2,2-trichloroacetimidate (1.53 g) in acetic acid (10 ml) was added a solution of 4-fluorobenzene-1,2-diamine in acetic acid (10 ml) under ice-cooling, followed by stirring at room temperature for 3 hours. The reaction liquid was concentrated under reduced pressure and to the obtained residue was added water, followed by neutralization with a saturated aqueous sodium hydrogen carbonate solution and extraction with EtOAc. The organic layer was washed with saturated brine, then dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from iPr2O/EtOAc/MeOH to obtain 5-fluoro-2-(trichloromethyl)-benzimidazole (1.5 g) as a beige powder.

The chemical industry reduces the impact on the environment during synthesis Methyl 2,2,2-trichloroacetimidate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Astellas Pharma Inc.; EP2351749; (2011); A1;,
Chloride – Wikipedia,
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57946-56-2, 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. 57946-56-2, name is 4-Chloro-2-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 5 Preparation of N-(4-chloro-2-fluorophenyl)-1-cyclohexene-1,2-dicarboximide A solution of 4-chloro-2-fluoroaniline (19.0 g, 130.6 mmol) and 3,4,5,6-tetrahydrophthalic anhydride (19.85 g, 130.6 mmol) in acetic acid is refluxed for 2 hours, treated with additional 4-chloro-2-fluoroaniline (3.0 g), refluxed for 90 minutes, stirred at room temperature overnight and poured into water. The resultant aqueous mixture is extracted with ethyl acetate. The organic extract is washed sequentially with water, saturated sodium hydrogen carbonate solution and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuoto obtain a purple oil. Flash column chromatography of the oil using silica gel and 15 to 20% ethyl acetate in hexanes solutions gives the title product as an off-white solid (25.3 g, 69% yield, mp 81-82C) which is identified by 1H, 13C and 19F NMR spectral analyses.

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

Reference:
Patent; American Cyanamid Company; EP985670; (2000); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 2163-00-0, These common heterocyclic compound, 2163-00-0, name is 1,6-Dichlorohexane, 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.

Examples 2 to 5; The procedure of Example 1 was repeated, except that the reaction of 1,6-dichlorohexane was carried out at a constant pH of 5, 6, 8 and 9. Before the start of the particular reaction, the weakly acidic mixture was adjusted to the pH of 5, 6, 8 and 9 with 2.5% sodium hydroxide solution (measurement with pH electrodes). Example 2 Example 3 Example 4 Example 5 pH value in 5.0 +/- 0.1 6.0 +/- 0.1 8.0 +/- 0.1 9.0 +/- 0.1 the reaction Residual 1,6-dichloro- <10 <10 <10 approx. 11 hexane content (ppm) Conversion of 1,6- >99.9 >99.9 >99.9 >99.9 dichlorohexane (%) In all examples (Examples 2 to 5), the resulting reaction mixture was clear and homogeneous. To determine the pure yield with respect to Examples 2 and 5, they were repeated once more. However, a GC analysis sample was not taken from the particular reaction mixture. The pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate was approx. 91.4%2) for the repetition of Example 2 and approx. 90.6%2) for the repetition of Example 5. 2) The pure yield for the synthesis according to Examples 2 and 5 was carried out again as in Example 1 by reacting the reaction solutions obtained in each case with aqueous NaBEC solution. In this procedure, the yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was approx. 89.6% of theory with a content of 95% for the reaction according to Example 2 and approx. 89.7% of theory with a content of approx. 94% for that according to Example 5. Thus, the pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate in the inventive reaction of 1,6-dichlorohexane with sodium thiosulphate pentahydrate must have been approx. 91.4% for the reaction according to Example 2 (89.6%×0.95×1/0.931=91.4%) and approx. 90.6% for that according to Example 5 (89.7%×0.94×1/0.931=90.6%).

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Buding, Hartmuth; US2005/240044; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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, Application In Synthesis of 2,4,5-Trifluorobenzene-1-sulfonyl chloride

[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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Related Products of 33786-89-9,Some common heterocyclic compound, 33786-89-9, name is 5-Chloro-m-phenylenediamine, molecular formula is C6H7ClN2, 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.

STR4 Using the above description one ordinarily skilled in the art can make and use the compounds of this invention. Specific embodiments of the invention are provided below. Structures and names of the embodied compounds are found summarized in CHART C. The examples below serve to illustrate the invention and are not intended to limit the invention in any manner. Example 1. Synthesis of N-(3-azido-5-ehlorophenyl)-N’-cyano-N”-(1,1dimethylpropyl)guanidine. Chart A. Step A-2. A stirred solution of 5-chloro-1,3-phenylenediamine (A-1, X is Cl, 1.93 g, 13.5 mmol) in 55 mL of dichloromethane is cooled to 0 C. and di-tert-butyl dicarbonate (2.96 g, 13.5 mmol) is added. The reaction mixture is stirred at 20-25 C. for 5 days and then concentrated. The residue is purified by medium pressure liquid chromatography using 25% ethyl acetate in hexane to afford 2.20 g of 3-amino-5-chlorophenylcarbamic acid, 1,1-dimethylethyl ester. (A-2) mp 85-87 C.; IR (mull) 3439, 3357, 3328, 2926, 1691, 1613, 1589, 1524, 1475, 1438, 1391, 1366, 1311, 1274, 1240, 1159, 851 cm-1; 1 H NMR (CDCl3) delta6.77 (bs, 1 H), 6.64 (m, 1 H), 6.39 (bs, 1 H), 6.34 (m, 1 H), 3.73 (bs, 2 H), 1.50 (s, 9 H); 13 C NMR (CDCl3) delta152.1, 147.8, 139.9, 134.8, 109.4, 108.2, 102.6, 80.5, 28.2; Analysis calculated for C11 H15 CIN2 O2: C, 54.44; H, 6.23; N, 11.54; Cl, 14.61. Found: C, 54.27; H, 6.50; N, 10.96; Cl, 13.99.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Chloro-m-phenylenediamine, its application will become more common.

Reference:
Patent; The Upjohn Company; US5525742; (1996); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 2267-25-6, name is 2-Chloro-4-fluoroanisole, molecular formula is C7H6ClFO, 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. Product Details of 2267-25-6

Sodium hydride (60% dispersion in mineral oil, 31 mg, 0.776mmol) was added to an ice- cooled solution of the product of preparation 20 (135mg, 0.388mmol) in N1N- dimethylformamide (4mL) and the mixture was stirred at O0C for 15 minutes. 2-chloro-4-fluoro- anisole (93mg, 0.582mmol) in N,N-dimethylformamide (1mL) was added and the mixture was stirred for 16 hours, at 5O0C. The solution was cooled to 250C and sodium hydride (60% dispersion in mineral oil, 62mg, 1.55mmol) was added and the solution was stirred for 16 hours at 80C. The reaction mixture was then cooled to 25C and quenched with water (3mL), concentrated in vacuo and the aqueous residue was partitioned between ethyl acetate (2OmL) and water (5mL). The aqueous layer was separated and extracted with ethyl acetate (2x20mL). The combined organic solution was washed with brine (1OmL), concentrated in vacuo and the residue was purified by column chromatography on silica gel, eluting with pentane: (ethyl acetate:methanol;0.88ammonia, 90:10:1), 3:1 to 1:1. The product containing fractions were evaporated under reduced pressure and the residue was further purified using an Isolute SCX-2 cartridge, eluting with methanol followed by 1M ammonia in methanol. The basic fractions were evaporated to afford the title compound as a yellow gum in 32% yield, 61mg.1HNMR(400MHz, CD3OD) delta: 1.03(s, 3H), 1.08(s, 3H), 1.28-1.31(m, 2H), 1.76-1.80(m, 1H), 1.86-1.93(m, 1H), 2.09-2.18(m, 1H), 2.49-2.63(m, 2H), 2.67-2.70(m, 1 H), 2.76-2.87(m, 2H), 3.80(s, 3H), 4.71-4.75(m, 1H), 6.74-6.77(dd, 1H), 6.89-6.95(dd, 1H), 7.24-7.46(m, 10H), 8.45- 8.59(m, 1 H); LRMS APCI m/z 489 [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 2267-25-6, its application will become more common.

Reference:
Patent; PFIZER LIMITED; WO2007/34325; (2007); A1;,
Chloride – Wikipedia,
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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. 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, A new synthetic method of this compound is introduced below., Computed Properties of C4H6Cl2

3-chloro-2-chloromethyl-1-propene (4.28 g), N, N-dimethylformamide (50 mL),To a mixture of sodium hydride (purity> 55%, 2.99 g),Under ice cooling, a solution of tert-butyl N- (2-hydroxypropyl) carbamate (5.00 g, CAS number: 95656-86-3) in tetrahydrofuran (20 mL) was added dropwise.The mixture was stirred at room temperature for 2.5 hours. After acetic acid (4.08 mL) was added to the reaction solution, water was added and the reaction mixture was extracted with ethyl acetate. Water organic layer,The extract was washed successively with saturated saline and dried over anhydrous magnesium sulfate.After filtration and concentration under reduced pressure, the obtained residue was subjected to silica gel column chromatography (n-hexane / ethyl acetate) three times,The title compound (2.61 g) was obtained as an oil.

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; Daiichi Sankyo Healthcare Co Ltd; Naito, Hiroyuki; Suzuki, Takayuki; Murata, Takeshi; Kawai, Junya; Higuchi, Saito; (99 pag.)JP2020/45306; (2020); A;,
Chloride – Wikipedia,
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These common heterocyclic compound, 2687-12-9, name is Cinnamyl 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. Computed Properties of C9H9Cl

General procedure: Aryl, benzyl or allyl halides (1.0mmol), arylboronic acid (1.2mmol), K2CO3 (1.5mmol), C1 (5×10-6 mol%) and H2O (2.0mL) were added into a sealed tube and the mixture was stirred at 60C for a few hours. After the reaction, the aqueous phase was extracted with ethyl acetate for 3 times (3×7mL). Then the combined organic layers were dried over anhydrous Na2SO4, concentrated under vacuum and purified by column chromatography.

The synthetic route of Cinnamyl chloride has been constantly updated, and we look forward to future research findings.

Reference:
Article; Luo, Kaixiu; Zhang, Lu; Yang, Rui; Jin, Yi; Lin, Jun; Carbohydrate Polymers; vol. 200; (2018); p. 200 – 210;,
Chloride – Wikipedia,
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