Month: July 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. 71510-95-7, name is Ethyl 3-(methylamino)-3-oxopropanoate, This compound has unique chemical properties. The synthetic route is as follows., name: Ethyl 3-(methylamino)-3-oxopropanoate

General procedure: In a round bottom flask, unsaturated aldehyde 2 (0.25 mmol, 1 equiv), amidomalonate 1 (0.3 mmol, 1.2 equiv), catalyst (0.05 mmol, 20% mol), and KOAc (0.3 mmol, 1.2 equiv) were added sequentially in 1 mL of 2,2,2-trifluoroethanol. The reaction was stirred at room temperature overnight. Then the crude was purified by column chromatography to furnish piperidine adducts 3.

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 71510-95-7.

Reference:
Article; ?ihalova, Sylva; Valero, Guillem; Schimer, Ji?i; Humpl, Marek; Dra?insky, Martin; Moyano, Albert; Rios, Ramon; Vesely, Jan; Tetrahedron; vol. 67; 46; (2011); p. 8942 – 8950;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 1103234-56-5, name is 2,6-Difluoro-3-(propylsulfonamido)benzoic acid, molecular formula is C10H11F2NO4S, 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 1103234-56-5

Example- 1 Preparation of 3-(Propane-l -sulfonylamino)-benzoyl chloride (IotaPi) Charge 2, 6-difiuoro-3-(((propan-l-yl) sulphonyl) amino) benzoic acid (5gm, 0.018 mol) was charged in to a reaction flask at 2S-30Ccontaining Toluene (25ml) under nitrogen atmosphere. Reaction mass was cooled to 10-15C. Thionyl chloride (15ml, 0.077mol) was added drop wise to mass at 10-15C and stirred for 15min. Reaction mass allowed to warm 25-30C and stirred for 30min. Heated the reaction mass to 105-110C and stirred for 4 hrs. Reaction mass cooled to 55-60C and organic volatiles distilled off completely to get semisolid residue and as such used in-situ for next stage.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1103234-56-5, its application will become more common.

Reference:
Patent; SHILPA MEDICARE LIMITED; PUROHIT, Prashant; NAGNNATH, Kokare; YENIREDDY, Veera Reddy; AKSHAY KANT, Chaturvedi; (0 pag.)WO2016/83956; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 39549-79-6,Some common heterocyclic compound, 39549-79-6, name is 2-Amino-4-methylbenzamide, molecular formula is C8H10N2O, 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 12mL vial was charged with MCM-41-2P-Pd(OAc)2 (2molpercent), 2-aminobenzamide (1mmol), aryl iodide (1mmol) (if solid) and a stirring bar. Then, DMF (2mL), aryl iodide (1mmol) (if liquid) and DBU (2mmol) were injected by syringe under an argon atmosphere. The vial was placed in an alloy plate, which was transferred into a 300mL Parr Instruments 4560 series autoclave under an argon atmosphere. After flushing the autoclave three times with CO, a pressure of 10bar CO was fixed at ambient temperature. The autoclave was heated for 20hat 120°C. After completion of the reaction, the autoclave was cooled to room temperature and the pressure was released carefully. The reaction mixture was diluted with ethyl acetate (10mL) and filtered. The palladium catalyst was washed with distilled water (2×5mL) and acetone (2×5mL), and reused in the next run. The filtrate was concentrated in vacuo and the pure product was isolated by either washed with water, ethyl acetate and finally hexane or recrystallization from MeOH.

The synthetic route of 39549-79-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; You, Shengyong; Huang, Bin; Yan, Tao; Cai, Mingzhong; Journal of Organometallic Chemistry; vol. 875; (2018); p. 35 – 45;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 122334-37-6, 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. 122334-37-6, name is 4-Chloro-N-methoxy-N-methylbenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation 2.2 6-(4-Chlorophenyl)-4-hydroxy-5-methyl-2H-pyran-2-one (IX) A suspension of 4.7 g of sodium hydride at 60% in oil, in 100 ml of THF, is cooled to 0 C. under a nitrogen atmosphere, a solution of 17 g of ethyl 3-oxopentanoate in 100 ml of THF is then added slowly, and the mixture is left to stir at 0 C. for 5 minutes. 86.5 ml of a 1.5 M solution of lithium diisopropylamide mono(tetrahydrofuran) in cyclohexane is then added dropwise at 0 C., and the mixture is left to stir at 0 C. for 20 minutes. Finally, a solution of 23.5 g of the compound of Preparation 1.2 in 50 ml of THF is added slowly and the mixture is left to stir while allowing the temperature to return to AT, and stirred overnight at AT. A mixture of ice/HCl at 10% is added, the reaction mixture is extracted with EtOAc, the organic phase is dried over Na2SO4, and the solvent is evaporated off under vacuum. The residue is taken up with 150 ml of concentrated H2SO4 and the mixture is left to stir at AT for 3 hours. The reaction mixture is poured onto ice and left to stir, and the precipitate formed is spin-filter-dried and washed with iso ether and then with pentane. 25 g of the expected compound are obtained after drying.

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, 4-Chloro-N-methoxy-N-methylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SANOFI-AVENTIS; US2009/281107; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 621-38-5, 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. 621-38-5, name is 3-Bromoacetanilide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Methyllithium (1.4 M in diethyl ether, 37.4 ml, 52.3 mmol) was added to a -78 C. solution of 3-bromoacetanilide (11.5 g, 53.7 mmol) in tetrahydrofuran (250 ml). The reaction was stirred 15 min at -78 C. Tert-butyllithium (1.7 M in pentane, 62.4 ml, 106 mmol) was added over 30 min to the -78 C. reaction mixture. The reaction was stirred 10 min at -78 C. N-methoxy-N-methyl (1-methyl(4-piperidyl))formamide (5.0 g, 26.8 mmol) in tetrahydrofuran (20 ml) was added dropwise to give a homogeneous yellow solution. The reaction mixture was stirred and allowed to warm to room temperature over 21 hours. The reaction mixture was cooled to 10 C., quenched with ice, and extracted with 1N hydrochloric acid solution. The aqueous extracts were washed with diethyl ether, basified to pH 12 with 5N sodium hydroxide solution and extracted with diethyl ether. The diethyl ether extracts were dried over sodium sulfate and the solvent was removed under reduced pressure to give 6.1 g of a yellow oil. The basic aqueous solution was again extracted with chloroform/isopropanol (3:1). These extracts were dried over sodium sulfate and the solvent was removed under reduced pressure to give 3.4 g of a yellow oil. Both oils were combined and purified by flash chromatography (silica gel, methylene chloride:methanol:ammonium hydroxide, 100:7.5:0.75) to yield 5.7 g (81%) of product as a yellow oil. [00418] MS(m/e): 261(M+1), 259(M-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, 3-Bromoacetanilide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Eli Lilly and Company; US6777428; (2004); B1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 78191-00-1, name is N-Methoxy-N-methylacetamide, 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 78191-00-1, Recommanded Product: 78191-00-1

5-methyl-thiazole (2.00g, 20.2mmol) was dissolved in tetrahydrofuran (50 mL) , at -78C, under nitrogen gas protection was slowly added dropwise n-butyl lithium (2.5M in tetrahydrofuran, 9.68mL, 24.2mmol). The reaction solution was stirred for 0.5 hours at -78C, and dissolved in tetrahydrofuran was slowly added dropwise (ImL) of N- methoxy -N- methyl-acetamide (2.50g, 24.2mmol). The reaction was warmed to 0C stirred for 1.5 h. At 0C slow addition of water (10mL) to the reaction mixture, and extracted with ethyl acetate(30mLx3) . The combined organic phase was dried over anhydrous sodium sulfate, filtered, and evaporated under reduced pressure, the obtained product was purified by preparative high performance liquid chromatography (1: 1 petroleum ether / ethyl acetate, Rf = 0.7) to give the product 1-(5-methylthiazol-2-yl)ethanone (1.45 g of, as a yellow solid), yield: 51%.

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

Reference:
Patent; Sichuan Gooddoctor Pharmaceutical Group Co., Ltd.; Wu, Lingyun; Zhang, Peng; Zhang, Li; Li, Jian; Chen, Shuhui; Geng, Funeng; Chen, Yongmei; Liu, Bin; Ma, Xiuying; (109 pag.)CN105566324; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 19962-04-0, These common heterocyclic compound, 19962-04-0, name is 3-Aminophenyl dimethylcarbamate, 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.

A. Preparation of tert-butyl 4-(tert-butoxycarbonylamino)-4-(3-(dimethylcarbamoyloxy)phenylcarbamoyl)piperidine-1-carboxylate. N-Boc-amino-(4-N-Boc-piperidinyl)carboxylic acid (0.114 g, 0.33 mmol), HATU (0.151 g, 0.40 mmol) and N,N-diisopropylethylamine (128 mg, 1.0 mmol) were combined in isopropyl acetate (2.3 mL) and stirred at room temperature for 15 minutes. 3-aminophenyl dimethylcarbamate (0.072 g, 0.40 mmol) was added, and the mixture heated at 80 C. for 1.5 hours. The reaction mixture was allowed to cool, diluted with EtOAc, washed with 2 N Na2CO3, 1 N HCl, and brine, and then dried over MgSO4 and concentrated. Purification by silica gel chromatography (60% EtOAc/hexanes) gave the title compound (0.075 g, 45%) as a white solid. MS (ES+) [M+NH4]+=524.

The synthetic route of 19962-04-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Burgoon, Hugh Alfred; Goodwin, Nicole Cathleen; Harrison, Bryce Alden; Healy, Jason Patrick; Liu, Ying; Mabon, Ross; Marinelli, Brett; Rawlins, David Brent; Rice, Dennis Stewart; Whitlock, Norris Andrew; US2009/264450; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 134575-14-7, name is exo-Benzyl 6-(hydroxymethyl)-3-azabicyclo[3.1.0]hexane-3-carboxylate, 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 134575-14-7, name: exo-Benzyl 6-(hydroxymethyl)-3-azabicyclo[3.1.0]hexane-3-carboxylate

24.2. (la,5a,6a)-6-Formyl-3-aza-bicyclo[3.1.0]hexane-3-carboxylic acid benzyl ester:DMP (15% in DCM, 20 mL) was added to a solution of intermediate 24.1 (1.27 g) in DCM (20 mL) at RT. After stirring for 2h40 at RT, sat. aq. NaHCO3 was added and the phases were separated. The org. phase was dried (MgSO^ and evaporated off. CC (Hept/EA 12/88 to EA) of the crude afforded 620 mg of the desired compound as orange oil.LC-MS: tR = 0.86 min; [M+H]+: 246.04.

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; ACTELION PHARMACEUTICALS LTD; CAROFF, Eva; HILPERT, Kurt; HUBLER, Francis; MEYER, Emmanuel; RENNEBERG, Dorte; WO2010/116328; (2010); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 75175-77-8, These common heterocyclic compound, 75175-77-8, name is 3-(4-Fluorophenyl)-N,N-dimethylacrylamide, 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: To a solution of the appropriate enaminone 2a-i (5 mmol) in glacial acetic acid (15 mL), ethyl acetoacetate (5.5 mmol) and ammonium acetate (40 mmol) were added. The reaction mixture was heated under reflux for 5 h. After cooling and pouring into ice-water, the residue obtained was filtered and washed with petroleum ether then with water and finally crystallized from ethanol [41]. The yields of compounds 3a-i were 80%, 77%, 81%, 84%, 86%, 80%, 785, 76%, 83%, respectively.

The synthetic route of 75175-77-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Eldehna, Wagdy M.; Fares, Mohamed; Abdel-Aziz, Marwa M; Abdel-Aziz, Hatem A; Molecules; vol. 20; 5; (2015); p. 8800 – 8815;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 209917-48-6, name is N-tert-Butyl 4-Aminophenylsulfonamide, molecular formula is C10H16N2O2S, 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 209917-48-6

Step 3; To a mixture of 4-amino-N-tert-butylbenzenesulfonamide (180 mg, 0.788 mmol, from step 2) and 3,3-dimethyl-2-oxobutanoic acid (308 mg, 2.4 mmol) in a 100 ml RBF at RT was added tetraisopropoxytitanium (2 ml,) via a pipet. The color of the mixture soon changed into a characteristic canary color. The solution was warmed to 75 C. for about 15 minutes and the color remained the same. The solution was diluted with absolute ethanol (8 ml) at RT, followed by the addition of 1.5× of sodium cyanotrihydroborate (245 mg, 3.90 mmol), and the remaining half after the bubbling and sizzling was over. The color of the solution became lighter. The solution was mixed with 4 mL of water, forming a suspension, and the white PPT was removed by centrifuge. The organic was extracted into ethyl acetate, and the organic phase was dried over Na2SO4, filtered, and evaporated to dryness. A yellow oil was obtained and was used directly in the next step without further purification. LC-MS, MS m/z 343 (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 209917-48-6, its application will become more common.

Reference:
Patent; Bristol-Myers Squibb Company; US2008/119461; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics