Author: tianli

3144-09-0, 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. 3144-09-0, name is Methylsulfonamide, This compound has unique chemical properties. The synthetic route is as follows.

In a 2-liter reaction flask, 1 liter of ethyl acetate and 66 grams of methylsulfonamide were added, and 109 grams of chloroacetyl chloride was gradually added; the temperature was gradually increased to 65C for 12 hours until the end of the reaction.The reaction solution gradually cooled to 0 degree, and a large amount of white solid precipitated; it was filtered and dried to obtain 112 g of solid SLP-10b (X=Cl).Yield: 94%.H NMR (400MHz, CDCl3): delta 4.02 (s, 2H), 3.28s, 3H)ESI/MS+(m/z):171

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; Shanghai Aikangrui Pharmaceutical Technology Co., Ltd.; Fan Linfeng; Zhu Yangwei; Qiu Aiyun; Lv Bojie; Xu Zhonghui; Zhang Changxuan; (11 pag.)CN106316967; (2017); A;,
Amide – Wikipedia,
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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. 17193-28-1, name is 1-Amino-1-cyclopentanecarboxamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 17193-28-1

General procedure: To a solution of protected proline (10 mmol) and triethylamine (1.40 ml; 10 mmol) in dry DCM (30 ml), ethyl chloroformate was added dropwise (0.95 ml; 10 mmol) in dry DCM (10 ml). After 30 min, aminoamide (10 mmol) in dry DCM (10 ml) was added to the mixture and the solution was stirred for 5 h. The organic layer was washed with water and aqueous sodium bicarbonate, dried over sodium sulfate and concentrated in vacuo. The residue was crystallised from the appropriate solvents.

The synthetic route of 17193-28-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Panov, Illia; Drabina, Pavel; Hanusek, Jiri; Sedlak, Milos; Tetrahedron Asymmetry; vol. 22; 2; (2011); p. 215 – 221;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

1882-71-9, Adding some certain compound to certain chemical reactions, such as: 1882-71-9, name is 2-Amino-5-methoxybenzamide, 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 1882-71-9.

General procedure: In a sealed tube equipped with a magnetic bar was charged with 2-amino benzamide derivatives (1, 3.67 mmol), cyclic 1,3-diones (2, 3.67 mmol) and TsOH.H2O (1.83mmol) in m-Xylene (5 mL). The reaction mixture was stirred at 150 ¡ãC for 8 h. After completion of the reaction, the reaction mass was cooled to room temperature, diluted with EtOAc, gave a water wash and the organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo. The crude product was purified by flash column chromatography (eluent: ethyl acetate/ n-hexane = 10?90) on silica gel to afford the desired product (4a-k).

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 1882-71-9.

Reference:
Article; Bingi, Chiranjeevi; Kola, Kaushik Yadav; Kale, Ashok; Nanubolu, Jagadeesh Babu; Atmakur, Krishnaiah; Tetrahedron Letters; vol. 58; 11; (2017); p. 1071 – 1074;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

326-67-0, A common heterocyclic compound, 326-67-0, name is N-(2-Fluoro-4-methylphenyl)acetamide, molecular formula is C9H10FNO, 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.

Chlorosulfonic acid(20.56 g,176.46 mmol,5 equiv.)was slowly added to N-(2-fluoro-4-methylphenyl)acetamide(5.90 g,35.29 mmol,1 equiv.)keeping the temperature of the reaction mixture below 50 C. The resulting mixture was then heated to 70 C for 4 hours. After cooling to room temperature,the reaction mixture was then poured carefully into ice,the precipitate was filtered,washed well with distilled water and dried to get 7.3 g of crude product as light brown solid. The crude product thus obtained was further used as such without any purification. NMR(CDCI3): delta 9.09(d,J = 7.6 Hz,1H),7.48(bs,1H),7.14(d, J = 10.8 Hz,1H),2.72(s,3H),2.25(s,3H).

The synthetic route of N-(2-Fluoro-4-methylphenyl)acetamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INSECTICIDES (INDIA) LIMITED; OAT AGRIO CO., LTD.; IMAI, Tetsuya; KUMAWAT, Surendra Kumar; SINGH, Manish Kumar; CHAUHAN, Pramod Kumar; BHATT, Ashish; SURAMWAR, Nikhil Vilas; SHELKE, Amol Vasant; SINGH, Rajesh Kumar; KISHORE, Ram; (138 pag.)WO2018/51252; (2018); A2;,
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Some common heterocyclic compound, 402-46-0, name is 4-Fluorobenzenesulfonamide, molecular formula is C6H6FNO2S, 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. 402-46-0

Example 10 27. N-(4-fluorobenzene)sulfonyl-alpha-dehydrovaline.; 3-methyl-2-oxobutyic acid, sodium salt (5.0 g, 36.2 mmol) was slurried in MTBE (25 mL) and cooled to 0 C, then HCI (12.1 N, 3.1 mL) was added. The resulting biphasic was warmed to rt, then saturated with Na2S04. The inorganic solids were filtered and washed with MTBE (25 mL). The combined organics were stripped to give a light-yellow oil. This oil was dissolved in toluene (35 mL) and diethyleneglycol diethyl ether (5 mL) and p-toluenesulfonamide (5.1 g, 29.0 mmol) then methanesulfonic acid (0.19 mL, 2.9 mmol) were added. The resulting mixture was heated at reflux with Dean-Stark removal of water for 24h, then cooled to 5 C. The resulting solid was filtered, and dried to give 5.4 g of crude material, which was recrystallized from MeOH/ water (16 mL/ 38 mL) to give 4.90 g of pure white solid (62% isolated yield). mp 172-173 C. IH-NMR (400 MHz, CD30D) d 7.83-7.86 (m, 2H), 7.22-7.27 (m, 2H), 2.12 (s, 3H), 1.87 (s, 3H); ?3C NMR (100 MHz, CD30D) 166.6,166.3, 163.7, 151.6, 136.7 (2 peaks), 129.9,129.8, 120.8, 115.5, 115.3, 22.0, 20.4 ppm. HRMS calcd for C11H11FNO4S (M-H) : 272.0393, Found: 272.0398.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 402-46-0, its application will become more common.

Reference:
Patent; MERCK & CO., INC.; WO2005/118529; (2005); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 144-80-9, name is N-((4-Aminophenyl)sulfonyl)acetamide, molecular formula is C8H10N2O3S, 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. 144-80-9

General procedure: 5.1.2.1. General procedure. A mixture of 2 (1.88 g, 0.01 mol) and sulfa-drugs (0.012 mol) in absolute ethanol (10 mL) and glacial acetic acid (5 mL) was refluxed for 21 h, then left to cool. The solid product formed was collected by filtration and recrystallized from ethanol-dimethylformamide to give 3-20.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 144-80-9, its application will become more common.

Reference:
Article; Ghorab, Mostafa M.; Alsaid, Mansour S.; Al-Ansary, Ghada H.; Abdel-Latif, Ghada A.; Abou El Ella, Dalal A.; European Journal of Medicinal Chemistry; vol. 124; (2016); p. 946 – 958;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

53297-70-4, 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. 53297-70-4, name is 4-Amino-3-methylbenzenesulfonamide, A new synthetic method of this compound is introduced below.

A cooled (0 0C) solution of e-chloropyhmidine^-carbonyl chloride (4.56 g; 25.8 mmol) in DCM (80 ml) was treated dropwise over 30 minutes with a solution of 4-amino-3-methyl-benzenesulfonamide (4.00 g; 21.5 mmol) and DIEA (7.40 ml; 43.0 mmol) in anhydrous DMF (10 ml_). At the end of addition the reaction mixture was concentrated under vacuum and the residue was taken up in EtOAc (200 mL). The organic phase was washed with water/brine (80 mL). A precipitate was formed, which was filtered and dried under vacuum to afford the crude product which was recrystallized from EtOH. The title product was obtained as a white solid. 1H NMR (300MHz, DMSO-d6) delta 10.65 (1 H, br s), 9.31 (1 H, d, J= 1.1 Hz), 8.24 (1 H, d, J= 1.1 Hz), 7.85-7.68 (3H, m), 7.33 (2H, br s), 2.36 (3H, s). MS (ESI-): 325.1. HPLC (Condition A): Rt 2.73 min (HPLC purity 100.0%).

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; LABORATOIRES SERONO SA; WO2009/19167; (2009); A1;,
Amide – Wikipedia,
Amide – 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 107017-73-2 as follows. 107017-73-2

Step 1 To a solution of tert-butyl (1-(hydroxymethyl)cyclopropyl)carbamate (Bioorg. Med. Chem. Lett., 2008, 18(6), 2188) (135 mg, 0.72 mmoles) in DCM (8 mL) was added Dess-Martin periodinane (277 mg, 0.65 mmole). After stirring 1 hr, the reaction was filtered through celite and concentrated to a yellow oil which was further purified by Isolera (7%-70% ethyl acetate/hexanes) to provide 84 mg (87%) of tert-butyl (l-formylcyclopropyl)-carbamate as a white solid.

According to the analysis of related databases, 107017-73-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Principia Biopharma Inc.; Goldstein, David Michael; US8673925; (2014); B1;,
Amide – Wikipedia,
Amide – 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. 239074-29-4, name is tert-Butyl (trans-4-(hydroxymethyl)cyclohexyl)carbamate, A new synthetic method of this compound is introduced below., 239074-29-4

To a solution of tert-butyl [trans-4-(hydroxymethyl)cyclohexyl]carbamate (0.50 g, 2.2 mmol) (Supplier: Chem-Impex) in methylene chloride (15 mL) was added triethylamine (1.29 mL, 9.27 mmol), 4-dimethylaminopyridine (53 mg, 0.44 mmol), and p-toluenesulfonyl chloride (0.89 g, 4.7 mmol). The resulting mixture was stirred at room temperature for 2 h before adding more p-toluenesulfonyl chloride (0.42 g, 2.2 mmol). The mixture was stirred overnight. Water and dichloromethane were added and the layers separated. The aqueous was extracted with dichloromethane. The combined organics were washed with water and brine, dried (MgSO4), filtered, and concentrated. The residue was purified on Biotage Isolera (40 g Agela cartridge, eluted with 5-50% EtOAc/hexanes over 15 min) to give the desired product (0.72 g, 86%) as a white crystalline solid. LCMS calculated for C19H29NO5SNa (M+Na)+: m/z=406.2. Found: 406.0.

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; Incyte Corporation; Li, Yun-Long; Zhu, Wenyu; Mei, Song; Glenn, Joseph; US2014/121198; (2014); 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. 57561-39-4, name is tert-Butyl (2-hydroxyethyl)(methyl)carbamate, This compound has unique chemical properties. The synthetic route is as follows., 57561-39-4

A 100 mL round-bottomed flask (rbf) equipped with a magnetic stirbar was charged withTHF (15 mL), water (15 mL) and 2-(methylamino)ethanol (2.00 mL, 25.0 mmol). To thestirred solution exposed to air Boc2O (5.9 g, 27 mmol) was added in 4 portions within 10min resulting in gas evolution. Several drops of sat. aq. NaHCO3 were added 40 min laterto keep the pH around 8. Most of THF was removed on a rotary evaporator 4.5 h after theBoc2O addition. The residue was transferred into a separatory funnel using EtOAc,washed with aq. 2.5 M NH4Cl (20 mL) and brine. The organic phase was dried overMgSO4, filtered into a 500 mL rbf and stripped of volatiles on the rotary evaporator.Using hexane transferred the crude product into a pre-weighed 100 mL rbf, removedvolatiles on the rotary evaporator (20 mm Hg). N-Methyl-N-Boc-aminoethanol wasobtained as colorless oil: 4.26 g (97%). A 3-neck rbf equipped with a magnetic stirbar, arubber septum, a glass stopcock (Teflon tape, central neck) and connected to a vacuumline was charged with 4.26 g of the protected amine (24.3 mmol). After evacuation andrefill with nitrogen 90 mL of THF freshly distilled from sodium-benzophenone ketyl wasadded. The flask was placed in an ice-water bath. Approx. 25 min later quickly added1.09 g of 60% NaH (27.2 mmol) in paraffin via the central neck. Approx. 20 min lateradded allyl bromide (2.15 mL, 24.8 mmol) with a syringe via the rubber septum followedby 0.4487 g of tetrabutylammonium iodide (1.21 mmol, 5 mol%) via the central neck.Approx. 2.5 h later removed the cold bath and let the reaction mixture stirring for 16 hunder nitrogen. The flask was immersed in ice-water bath followed by careful addition ofwater (20 mL, audible sound). The mixture was transferred into a 250 mL separatoryfunnel followed by addition of EtOAc (50 mL) and extraction. The organic phase was setaside and the aqueous phase was extracted with fresh portion of EtOAc (40 mL). Theorganic phases were combined, washed with aq. 2.5 M NH4Cl (50 mL) and brine, driedover MgSO4, filtered into a 500 mL rbf and stripped of volatiles on the rotary evaporatorleaving behind yellow oil, which was chromatographed on silica (normal phase, EtOAchexane,1:3) furnishing 3.7916 g of N-Methyl-N-Boc-aminoethanol O-allyl ether ascolorless oil (72% yield). N-Boc deprotection was achieved according to the method ofStrazzolini et al.1 To a 200 mL rbf charged with a magnetic stirbar and CH2Cl2 (22 mL)and immersed in an ice-water bath added 1.48 mL of conc. H2SO4 (assumed to be 17.9 M,26.5 mmol) with stirring. The central neck was plugged with a glass stopcock while adropping funnel was attached to the side-neck. A solution of 3.79 g of N-Methyl-N-BocaminoethanolO-allyl ether (17.6 mmol) in 65 mL CH2Cl2 was added to the solution ofacid dropwise from the addition funnel within 45 min followed by removal of cold bathand stirring at rt for 6 h. The dark purple mixture was transferred into a separatory funneland extracted with water (40 mL). The organic phase was extracted with additional 40mL of water, after which the aqueous extracts were combined in a 200 mL Erlenmeyerflask and basified by addition of NaOH (3.245 g in 15 mL water) with stirring. Theresulting solution was saturated with NaCl and extracted with three 50 mL portions ofCH2Cl2. Combined extracts were dried over Na2SO4, filtered into a 500 mL rbf andstripped of the solvent on the rotary evaporator (200 mm Hg). The resulting yellowish oilwas fractionated in vacuo using a one-piece distillation head and a receiving flask held at-50 C. The title compound was obtained as colorless oil (1.2208 g, 60% yield).

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; Kultyshev, Roman G.; Miyazawa, Akira; Tetrahedron; vol. 67; 11; (2011); p. 2139 – 2148;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics