Month: July 2021

Adding a certain compound to certain chemical reactions, such as: 6325-93-5, name is 4-Nitrobenzenesulfonamide, belongs to amides-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 6325-93-5, COA of Formula: C6H6N2O4S

Step 1 – Tert-butyl N-(4-nitrophenyl)sulfonylcarbamate (0596) [00375] To a solution of 4-nitrobenzenesulfonamide (5.00 g, 24.7 mmol) in anhydrous dichloromethane (40 mL) was added triethylamine (5.00 g, 49.4 mmol) and catalytic amount of N,N-dimethylpyridin-4-amine. The mixture was cooled to 0 C and di-tert-butyl dicarbonate (5.67 g, 25.9 mmol) was added over 10 min. Then the mixture was warmed to 18 C and stirred for 50 min. On completion, the reaction mixture was quenched with ice water (40 mL). Afterwards, the organic phase was separated, washed with brine (20 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to give a residue. The residue was purified by column chromatography (petroleum ether:ethyl acetate = 3:1 to 1:1) to give the title compound.1H NMR (400MHz, CDCl3) delta = 8.44 – 8.40 (m, 2H), 8.28 – 8.24 (m, 2H), 1.43 (s, 9H).

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; RAZE THERAPEUTICS, INC.; MAINOLFI, Nello; MOYER, Mikel P.; SAIAH, Eddine; (264 pag.)WO2017/156181; (2017); A1;,
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Adding a certain compound to certain chemical reactions, such as: 1259224-00-4, name is tert-Butyl (1-(4-aminophenyl)cyclobutyl)carbamate, belongs to amides-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 1259224-00-4, Safety of tert-Butyl (1-(4-aminophenyl)cyclobutyl)carbamate

To the solution of 2,4-Dichloro-6-methyl-5-nitro-pyrimidine (2.08 g, lO.OOmmol) in THF (50 mL) at -78 C was slowly added the solution of [l-(4-Amino-phenyl)- cyclobutyl]-carbamic acid tert-butyl ester (2.62 g, 10.00 mmol) in THF (20 mL). The reaction mixture was stirred at ambient temperature for 30 min.. Then it was concentrated to remove the solvent. The obtained residue was dissolved in ethyl acetate (250 mL) and washed by saturated. NaHC03 solution, followed by brine. The separated organic layer was dried over sodium sulfate, filtered and concentrated to give { l-[4-(2-Chloro-6-methyl-5-nitro-pyrimidin-4-ylamino)-phenyl]- cyclobutyl}-carbamic acid tert-butyl ester. (4.3 g, 98%yield). MS (ESI+) e/z: 370.9 / 372.9 [M+l]+.

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; ARRAY BIOPHARMA INC.; GENENTECH, INC.; SKELTON, Nicholas; GRADL, Stefan; BLAKE, James F.; GRAHAM, James M.; GUNAWARDANA, Indrani W.; HENTEMANN, Martin; MARLOW, Allison L.; TANG, Tony P.; WO2013/78254; (2013); A1;,
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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. 1015-89-0, name is Phenanthridin-6(5H)-one, A new synthetic method of this compound is introduced below., SDS of cas: 1015-89-0

The 5,6-dihydro-phenanthridine (Ik) was prepared using the following procedure: Into a 500 mL round bottom flask equipped with a magnetic stir bar and a reflux condensor was placed 6(5H)-Phenanthridinone (1000 mg, 5123 mumol), THF (250 mL) (fine suspension). The flask is sparged with nitrogen, 2M BH3-dimethylsulfide complex in THF (10 mL) is added. This is allowed to stir at reflux for 24 hours. TLC shows reaction still incomplete (1/1, ethyl acetate/heptane). Solvents removed under reduced pressure. Water (50 mL) and ethyl acetate (100 mL) added. The aqueous layer is separated with ethyl acetate (3 x 100 mL). The organic layers are combined, dried(sodium sulfate), solids removed by filtration, and the solvents removed under reduced pressure. This is purified by silica column chromatography using heptane to 50percent ethylacetate in heptane. The best fractions are pooled and the solvents are removed under reduced pressure to afford an off-white solid (270 mg, Yield: 29percent). LC-MS shows mass 182 (M+H)+.

The synthetic route of 1015-89-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TIBOTEC PHARMACEUTICALS LTD.; MEDIVIR AB; WO2008/96001; (2008); A1;,
Amide – Wikipedia,
Amide – 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. 2618-96-4, name is Dibenzenesulfonimide, This compound has unique chemical properties. The synthetic route is as follows., category: amides-buliding-blocks

General procedure: To a solution of N-sulfonylsulfonamide 1 (1.68 mmol) in N,N-disubstituted formamide 3 (3.0 mL) was added TsCl (2; 0.160 g, 0.840 mmol; 0.480 g, 2.52 mmol for products 4d-g) and Et3N (0.29 mL, 2.10 mmol). The mixture was stirred at r.t. (or heated to 100 C in the cases of 4d-g,k). After the starting material was consumed as indicated by TLC, the reaction mixture was poured into H2O and extracted with CH2Cl2. The combined organic phases were washed with H2O, dried (anhydrous MgSO4), filtered, and concentrated under reduced pressure. The crude product was purified, if necessary, by silica gel flash column chromatography (hexane/EtOAc) to give the desired product as a white solid (Table 2).

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 2618-96-4.

Reference:
Article; Jeong, Yuri; Ban, Jaeyoung; Lim, Minkyung; Rhee, Hakjune; Synthesis; vol. 50; 9; (2018); p. 1867 – 1874;,
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Synthetic Route of 2618-96-4, The chemical industry reduces the impact on the environment during synthesis 2618-96-4, name is Dibenzenesulfonimide, I believe this compound will play a more active role in future production and life.

Iodobenzene diacetate(579.8 mg, 1.8 mmol)And bis (benzenesulfonyl) imide(535.23 mg, 1.8 mmol) was added toIn acetonitrile,The mixture was stirred at 40 C. for 30 minutes.After that, N-pivaleindole (301.9 mg, 1.5 mmol) was added toAnd the mixture was stirred at room temperature for 3 hours.After removal of the solvent, ether was added,Filter,Washed with ethyl acetate,1- (2,2-Dimethyl-1-oxopropyl)-3- [bis(Benzenesulfone)Amidyl](Phenyl)-lambda 3 -iodanyl]-1 H-indole(893.28 mg, 85%).

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, Dibenzenesulfonimide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chiba University; Moriyama, Katsuhiko; Togo, Hideo; Ishida, Kazuma; (40 pag.)JP2015/34144; (2015); A;,
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Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 127-77-5, name is 4-Amino-N-phenylbenzenesulfonamide, molecular formula is C12H12N2O2S, 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. HPLC of Formula: C12H12N2O2S

To a well-stirred solution of compound 2 (2.48 g, 0.01 mol) inchloroform, benzoyl chloride (1.28 ml, 0.011 mol) in chloroformwas added dropwise at 0 C and stirring was continued in cold condition.After the completion of reaction (monitored by TLC), thereaction mixture was poured into ice cold water. White solid wasfiltered, washed with acetic acid and sodium bicarbonate solutions,dried and purified by recrystallization. Single crystals suitable fordiffraction studies were obtained by slow evaporation fromethanol.Analytical and physical data: Formula: C19H16N2O3S; Yield:70-75%; LCMS (+ve mode): (M + H) = 353.0 (99.5%), RT – 4.349;HRMS: Obtained m/z = 375.0777 (M + Na), cald. = 375.0779.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 127-77-5, its application will become more common.

Reference:
Article; Lahtinen, Manu; Kudva, Jyothi; Hegde, Poornima; Bhat, Krishna; Kolehmainen, Erkki; Nonappa; Venkatesh; Naral, Damodara; Journal of Molecular Structure; vol. 1060; 1; (2014); p. 280 – 290;,
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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. 17641-08-6, name is 2-Chloro-N-(3-methoxyphenyl)acetamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 2-Chloro-N-(3-methoxyphenyl)acetamide

General procedure: To a stirred solution of substituted aniline (1 mmol) and chloroacetyl chloride (1 mmol) which was stirred in 5 mL DMF for 20 min, were added benzyl amine derivatives (1.3 mmol) and CS2 (5 mmol). The reaction mixture was allowed to stir for required additional time (Table 2). Then, 5 mL of water was added and the solution was extracted with ethyl acetate and dried over sodium sulfate and purified by passing over a silica gel column chromatography using petroleum ether/ethyl acetate (8:2).

The synthetic route of 17641-08-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sadat-Ebrahimi, Seyed Esmail; Karim, Leila; Moghimi, Setareh; Yahya-Meymandi, Azadeh; Mahdavi, Mohammad; Vosooghi, Mohsen; Foroumadi, Alireza; Shafiee, Abbas; Journal of Sulfur Chemistry; vol. 38; 1; (2017); p. 43 – 51;,
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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 25625-57-4 as follows. Quality Control of 2-Bromo-N-(3-(trifluoromethyl)phenyl)acetamide

Example 5: 2-[3-(4-Bromophenyl)-2-oxo-7-oxa-1 ,4-diazaspiro[4.5]dec-3-en-1 -yl]-N-[3- (trifluoromethyl)phenyl]acetamide; 3-(4-Bromophenyl)-7-oxa-1 ,4-diazaspiro[4.5]dec-3-en-2-one (D19) (100mg, 0.32mmol) in DMF (4ml) was cooled to ice bath temp and treated with sodium hydride (14.23 mg, 0.356 mmol) under an atmosphere of argon. The mixture was stirred for 30 minutes then 2- bromo-N-[3-(trifluoromethyl)phenyl]acetamide (D16) (100 mg, 0.356 mmol) in DMF (2ml) was added over 1.5 hour by syringe pump. The mixture was then allowed to warm to room temp overnight. The mixture was poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with brine and dried using sodium sulphate and the solvent was removed. The residue was chromatographed on a silica column eluted with a gradient of 0-5% methanol in DCM. A mixture was obtained which was purified by low pH MDAP to give the title compound (81 mg).1H NMR (d6DMSO) delta: 1.65-1.80 (2H, m), 2.06-2.28 (2H, m), 3.5 (1 H, m), 3.65 (1 H, m), 3.8-3.95 (2H, m), 4.5 (2H, m), 7.42 (1 H, m), 7.61 (1 H, m), 7.77 (3H, m) 8.08 (1 H, m), 8.32 (2H, s), 10.6 (1 H, s). 19F NMR (DMSO) delta: -61.4 (s), Mass Spectrum (Electrospray LC/MS): Found 510 (MH+). Ret. time 3.33 min.

According to the analysis of related databases, 25625-57-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXO GROUP LIMITED; UNIVERSITY OF NOTTINGHAM; WO2008/92877; (2008); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 14433-76-2, The chemical industry reduces the impact on the environment during synthesis 14433-76-2, name is N,N-Dimethylcapramide, I believe this compound will play a more active role in future production and life.

Comparative example AIn the same reactor set up, example 1 is repeated except for the DMA addition. The selectivity towards N,N-dimethyldecylamine is reduced to 92.5 %, mainly at expense of N-methyldidecylamine and decanol.

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

Reference:
Patent; TAMINCO; WO2006/136204; (2006); A1;,
Amide – Wikipedia,
Amide – 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. 563-83-7, name is Isobutyramide, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C4H9NO

Intermediate 1: 2-Methylpropanethioamide; A solution of 2-methylpropanamide (6.53 g, 75.0 mmol) and 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (15.17 g, 37.51 mmol) in THF (100 mL) was heated to reflux for 4 h. The reaction mixture was then cooled to rt and poured into saturated aqueous NaHCO3 (200 mL). The mixture was extracted with ether (4×100 mL). The organic fractions were combined, dried over Na2SO4, filtered, and concentrated. Purification by flash column chromatography (20% EtOAc:hexanes) afforded 4.77 g (62%) of the title compound. 1H-NMR (400 MHz, CDCl3) delta 7.63 (brs, 1H), 6.90 (brs, 1H), 2.88 (m, 1H), and 1.27 (d, 6H, J=6.8 Hz).

According to the analysis of related databases, 563-83-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Adams, Jerry Leroy; Dickerson, Scott Howard; Johnson, Neil W.; Kuntz, Kevin; Petrov, Kimberly; Ralph, Jeffrey M.; Rheault, Tara Renae; Schaaf, Gregory; Stellwagen, John; Tian, Xinrong; Uehling, David Edward; Waterson, Alex Gregory; Wilson, Brian; US2009/298815; (2009); A1;,
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Amide – an overview | ScienceDirect Topics