Tag: M.W=0-100

Reference of 598-55-0, 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. 598-55-0, name is Methyl carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a mixture of 2-naphthol(5 mmol), an aldehyde (5 mmol), and a carbamate(5.5 mmol), CuCl2·2H2O (0.05 mmol) was added. Thereaction mixture was stirred on a preheated water bathat 70C. After completion of the reaction (monitoredby TLC), the reaction mixture was cooled to RT.washed with H2O/EtOH (v/v = 1/1), and recrystallizedfrom H2O/EtOH (v/v = 2/3). The products were characterized by IR, 1H NMR, 13C NMR, LC/MS andelemental analysis.

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, Methyl carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Song, Zhiguo; Liu, Lianli; Sun, Xiaohu; Cui, Yan; Indian Journal of Chemistry – Section B Organic and Medicinal Chemistry; vol. 53; 6; (2014); p. 740 – 745;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 6228-73-5, 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. 6228-73-5, name is Cyclopropanecarboxamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a microwave tube was added7-chloro-2-(2,6-dichlorophenyl)thieno[2,3-c]pyridine(150 mg, 0.48 mmol),cyclopropanecarboxamide(81 mg, 0.95 mmol), Pd2(dba)3(22 mg, 0.024 mmol), XantPhos (28 mg, 0.048 mmol), Cs2CO3(311 mg, 0.95 mmol) and dioxane (4 mL).The mixture was degassed with N2for 10 min. The resulting mixture was irradiated in a microwave reactor at 150 C for 1.5 h and then cooled to room temperature. The mixture was filtered throughCeliteand the filtrate was concentrated. The residue was purified by silica gel column chromatography eluting with a 0-60% gradient ofEtOAcin dichloromethane to afford a solid. The solid was triturated with diethyl ether and collected by filtration to afford the title compound (110 mg, 64% yield). H NMR (300 MHz, CDCl3):delta 8.96 (1H,brs), 8.21 – 8.17 (1H, m), 7.55 (1H, d,J= 5.5 Hz), 7.45 – 7.41 (2H, m), 7.35-7.24 (2H, m), 1.24 – 1.15 (3H, m), 0.99 – 0.91 (2H, m); LCMS (ESI) m/z: 363.2 [M+H]+.HRMS m/z [M+H]+calcd.forC17H12Cl2N2OS 363.0125, found 363.0118.

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

Reference:
Article; Liang, Jun; Van Abbema, Anne; Balazs, Mercedesz; Barrett, Kathy; Berezhkovsky, Leo; Blair, Wade S.; Chang, Christine; Delarosa, Donnie; DeVoss, Jason; Driscoll, Jim; Eigenbrot, Charles; Goodacre, Simon; Ghilardi, Nico; MacLeod, Calum; Johnson, Adam; Bir Kohli, Pawan; Lai, Yingjie; Lin, Zhonghua; Mantik, Priscilla; Menghrajani, Kapil; Nguyen, Hieu; Peng, Ivan; Sambrone, Amy; Shia, Steven; Smith, Jan; Sohn, Sue; Tsui, Vickie; Ultsch, Mark; Williams, Karen; Wu, Lawren C.; Yang, Wenqian; Zhang, Birong; Magnuson, Steven; Bioorganic and Medicinal Chemistry Letters; vol. 27; 18; (2017); p. 4370 – 4376;,
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. 563-83-7, name is Isobutyramide, A new synthetic method of this compound is introduced below., Application In Synthesis of Isobutyramide

General procedure: Acetone (5.0 mL) was added to the mixture of amide (2.0 mmol) and aldehyde (1.0mmol), followed by the addition of BF3 etherate (12.6 muL, 0.1 mmol).Then the mixture was stirred at room temperature until the full consumption ofstarting material detected by TLC analysis. Then the product was collected assolid by filtration and washed with a small portion of diethyl ether. After drying under vacuum, the purity was checked by 1HNMR: only desired peaks were observed except minor solvent residue in only afew cases.

The synthetic route of 563-83-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Yi; Zhong, Zhihao; Han, Yingmei; Han, Ruirui; Cheng, Xu; Tetrahedron; vol. 69; 52; (2013); p. 11080 – 11083;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 6228-73-5, 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. 6228-73-5, name is Cyclopropanecarboxamide, This compound has unique chemical properties. The synthetic route is as follows.

Cyclopropanecarboxamide (58.7g, 690 mmol) in 1,4-Dioxane (1600 ml) was added 2-bromoacetyl bromide (59.9 ml, 690 mmol) at room temperature and stirred for 4h at 600C. The reaction mixture was concentrated to dryness. The residue was dissolved in EtOAc and carefully washed with satd. NaHCObeta, water then with brine solution, dried over Na2SO4 and concentrated to get N-(2- bromoacetyl) cyclopropanecarboxamide(138 g, 670 mmol, 97 % yield) as an off white solid. This material was used without purification. ESI-MS :m/z 208.0 (M+2H)+.

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

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; BRESSI, Jerome, C.; CHU, Shaosong; ERICKSON, Philip; KOMANDLA, Mallareddy; KWOK, Lily; LAWSON, John, D.; STAFFORD, Jeffrey, A.; WALLACE, Michael, B.; ZHANG, Zhiyuan; DAS, Sanjib; WO2010/19899; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 563-83-7, These common heterocyclic compound, 563-83-7, name is Isobutyramide, 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 solution of 38 phosphorus pentasulfide (P2S5) (4.58mmol) in ether (8ml) was added 39 isobutylamide 11a (1gm, 11mmol) and the reaction mixture was stirred for 2h at room temperature. The reaction mixture was diluted with brine and extracted with ether. The organic layer was dried over Na2SO4 and evaporated to give crude 40 thioamide. The mixture of crude 40 thioamide and 42 ethyl alpha-bromopyruvate (11.42mmol) in 43 EtOH (10ml) was stirred at reflux temperature for 30min. The solvent was evaporated under vacuum, diluted with EtOAc and washed with 7% aqueous NaHCO3 (3×30mL), the organic layer was dried over Na2SO4 and evaporated to get crude product, which was purified by column chromatography (n-hexane/EtOAc) to afford 44 12a.

Statistics shows that Isobutyramide is playing an increasingly important role. we look forward to future research findings about 563-83-7.

Reference:
Article; Karale, Uttam B.; Krishna, Vagolu Siva; Krishna, E. Vamshi; Choudhari, Amit S.; Shukla, Manjulika; Gaikwad, Vikas R.; Mahizhaveni; Chopra, Sidharth; Misra, Sunil; Sarkar, Dhiman; Sriram, Dharmarajan; Dusthackeer, V.N. Azger; Rode, Haridas B.; European Journal of Medicinal Chemistry; vol. 178; (2019); p. 315 – 328;,
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 631-58-3 as follows. Product Details of 631-58-3

0.40 g (1 .47 mmol) 5-bromo-azepan-4-one hydrobromide, 0.13 g (1 .47 mmol) thiopropionamide and 3 mL ethanol. were stired under reflux for 3 hours. The reaction was allowed to cool to RT and was filtered. The filtrate was concentrated to dryness and dried. Yield: 0.39 g (quantitativ) ESI-MS: m/z = 183 (M+H)+ Rt(HPLC): 0.39 min (Method J)

According to the analysis of related databases, 631-58-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; GOTTSCHLING, Dirk; EBEL, Heiner; RIETHER, Doris; WELLENZOHN, Bernd; WO2013/144172; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 15910-91-5, name is 1-Methylcyclopropanecarboxamide, 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 15910-91-5, Formula: C5H9NO

Bromine (2. 87mol, 0. 056mol) was added to a solution of sodium hydroxide (13. 5g, 0. 338mol) in water (100ml) at 0-5 C. A slurry of 1- (1-methylcyclopropane) carboxamide (Method 51 ; 5.70g 0. 056mol) in water (sol) was then added and reaction mixture stirred at 5 C for 2 hours, then left to stand at ambient temperature for 24 hours. The mixture was then heated at 80 C for 2.5 hours, allowed to cool and mixture distilled to give the title compound (bp 75-80 C). NMR : 0.2 (q, 2H), 0.14 (q, 2H), 0.96 (s, 3H), 1.42 (s, 2H).

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; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2003/76436; (2003); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 6228-73-5, name is Cyclopropanecarboxamide, 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. SDS of cas: 6228-73-5

Step 1 : 4-(Chloromethyl)-2-cyclopropylthiazole[0174] To a slurry of cyclopropanecarboxamide (10 g, 0.12 mol) in MTBE (150 rnL) was charged P2S5 (5 g, 12 mmol). The mixture was heated to 100 0C for 2 h (monitored by TLC, EtOAc/hexane 1 :1) and cooled to room temperature. Supernatant was decanted and concentrated to afford the intermediate thioamide (6 g, 56%) as a light yellow solid. MS (ES) m/z 102.1 (M+ H+)). This was suspended in acetone (100 mL) and charged with 1,3- dichloroacetone (7.0 g, 0.055 mol). The mixture was heated to reflux for 8 h (monitored by TLC, EtOAc/hexane 1 :1), cooled to room temperature and concentrated. The residue was purified by silica gel chromatography using 2 to 10% EtOAc in hexane to afford the title compound (8.0 g, 79%) as a light brown oil. 1H NMR (400 MHz, CDCl3) delta 7.02 (s, IH), 4.62 (s, 2H), 2.32 (m, IH), 1.16 (m, 2H), 1.05 (m, 2H). MS (ES) m/z 174.1 (M+ H+).

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

Reference:
Patent; CHEMOCENTRYX, INC.; CHEN, Xi; FAN, Pinchen; GLEASON, Mark, M.; JAEN, Juan, C.; LI, Lianfa; MCMAHON, Jeffrey, P.; POWERS, Jay; ZENG, Yibin; ZHANG, Penglie; WO2010/54006; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 7341-96-0, 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. 7341-96-0, name is Propiolamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The imine (0.2mmol), rhodium acetate (0.002mmol), Molecular sieve (300 mg) and the mixture is dissolved 1.5 ml dichloromethane solvent, into mixed solution 1, in 20 C stirring for 10 minutes. Then the propargyl amide (0.24mmol) and phenyl diazonium acetic acid methyl ester (0.24mmol) dissolved in 1.0 ml methylene chloride solvent, into solution 2. The solution 2 for 20 C lower, in 1 hour for adding and mixing the solution in the injection pump 1. The reaction mixture is purified by rapid column chromatography, to obtain the pure product, its structure is shown as formula (f) is shown. The yield is 89%, dr value is equal to the 88:12. The product of the1As shown in Figure 11, H NMR schematic view thereof13C NMR schematic view as shown in Figure 12.

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

Reference:
Patent; EAST CHINA NORMAL UNIVERSITY; HU, WENHAO; WU, YONG; WANG, WENKE; TANG, MIN; (29 pag.)CN106146334; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 3144-09-0, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 3144-09-0 name is Methylsulfonamide, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

8.4 g (0.02 mol) of 2-{4-[N-(5,6-diphenylpyrazin-2-yl)-N-isopropylamino] butyloxy} acetic acid and 60 mL of dichloromethane were added into a 100 mL flask and cooled to 5 C., 3.8 g (0.03 mol) of oxalyl chloride was added dropwise, then reacted at room temperature for 2 hours, the solvent was concentrated to dryness, 50 mL of acetonitrile was added to dissolve, and the X4 solution was obtained as a stand-by. (0077) 2.85 g of methanesulfonamide, 20 mL of acetonitrile and 3 g of triethylamine were added into another flask and cooled to 10 C., the X4 solution obtained above was added dropwise, then reacted at this temperature for 5 hours, until the reaction was completed. (0078) The finished reaction solution was poured into 100 mL of ice water, the mixture was extracted with ethyl acetate, the solvent of the organic phase was concentrated to dry, the residue was recrystallized with ethanol, and 8.8 g off-white crystals of NS-304 was obtained, the molar yield was 88%, HPLC purity was 99.5%. (0079) 1H-NMR data: 1H-NMR (400 MHz, CDCl3) delta: 8.19 (s, 1H), 7.44 (m, 2H), 7.35 (m, 2H), 7.30-7.21 (m, 6H), 3.97 (s, 2H), 3.59 (t, J=6.0 Hz, 2H), 3.45 (t, J=6.8 Hz, 2H), 3.29 (s, 3H), 1.75-1.70 (m, 4H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methylsulfonamide, and friends who are interested can also refer to it.

Reference:
Patent; Seasons Biotechnology (Taizhou) Co., Ltd.; TANG, Fanghui; MA, Chi; JIA, Qiang; (11 pag.)US2018/29998; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics