Author: Jessica.F

Related Products of 5238-56-2, The chemical industry reduces the impact on the environment during synthesis 5238-56-2, name is N-(2-Hydroxyethyl)methacrylamide, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of glycosyl donor10 1 (0.635 gm, 1 mmol), glycosyl acceptor 10b (0.142 g 1.1 mmol) and 4 A molecular sieves powder (100 mg) in anhydrous CH2Cl2 (10 mL) was added AuBr3 (0.031 g, 0.07 mmol) under argon atmosphere at room temperature. The reaction mixture was stirred at room temperature for the specified time and the completion of the reaction is judged by TLC analysis. The reaction mixture was filtered through Celite and the filtrate was concentrated in vacuo to obtain a crude residue which was purified by conventional silica gel column chromatography using ethyl acetate-petroleum ether as mobile phase to obtain compound 11b.

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-(2-Hydroxyethyl)methacrylamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Thadke, Shivaji A.; Kar, Mritunjoy; Gupta, Sayam Sen; Hotha, Srinivas; Carbohydrate Research; vol. 346; 12; (2011); p. 1511 – 1518;,
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Application of 17641-08-6,Some common heterocyclic compound, 17641-08-6, name is 2-Chloro-N-(3-methoxyphenyl)acetamide, molecular formula is C9H10ClNO2, 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 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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366-49-4, name is 2-Acetamido-4-fluorotoluene, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 366-49-4

A solution of 5-fluoro-2-methylaniline (25 g, 200 mmol) in toluene (250 mL) was treated with Ac2O (25 mL, 226 mmol) and heated at reflux for 1 h. The reaction mixture was concentrated in vacuo when a colorless solid precipitated out which was filtered and washed with ether and hexanes. The colorless solid was taken in acetic acide (150 mL) and treated with a solution of Br2 (9.6 mL, 186 mmol) in acetic acid (20 mL) and stirred at rt for 12 h. The reaction mixture was diluted with water when a colorless solid 17 (40 g, 81.6%) precipitated out. It was filtered and extensively washed.

The synthetic route of 366-49-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Venkatraman, Srikanth; Velazquez, Francisco; Gavalas, Stephen; Wu, Wanli; Chen, Kevin X.; Nair, Anilkumar G.; Bennett, Frank; Huang, Yuhua; Pinto, Patrick; Jiang, Yueheng; Selyutin, Oleg; Vibulbhan, Bancha; Zeng, Qingbei; Lesburg, Charles; Duca, Jose; Heimark, Larry; Huang, Hsueh-Cheng; Agrawal, Sony; Jiang, Chuan-Kui; Ferrari, Eric; Li, Cheng; Kozlowski, Joseph; Rosenblum, Stuart; Shih, Neng-Yang; George Njoroge; Bioorganic and Medicinal Chemistry; vol. 22; 1; (2014); p. 447 – 458;,
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Reference of 6973-09-7,Some common heterocyclic compound, 6973-09-7, name is 5-Amino-2-methylbenzenesulfonamide, molecular formula is C7H10N2O2S, 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.

2-Chloro-5-fluoro-N4-[4-(prop-2-ynyloxy)phenyl]-4-pyrimidineamine (0.514 g, 1.85 mmol), 3-(aminosulfonyl)-4-methylaniline (0.689 g, 3.70 mmol, made by reduction of commercially available 2-methyl-5-nitrobenzenesulfonamide or synthesized as described below), and trifluoroacetic acid (0.186 mL, 2.41 mmol) were combined with iPrOH (6.0 mL) in a sealed vial and heated at 100¡ã C. for 3 h. The reaction mixture was cooled to room temperature and diluted with 1N HCl (80 mL). N2-(3-Aminosulfonyl-4-methylphenyl)-5-fluoro-N4-[4-(prop-2-ynyloxy)phenyl]-2,4-pyrimidinediamine (I) was isolated as a white solid by suction filtration (0.703 g). 1H NMR (DMSO-d6): delta 10.08 (bs, 2H), 8.19 (d, J=4.5 Hz, 1H), 7.89 (s, 1H), 7.74 (dd, J=2.4 and 8.4 Hz, 1H), 7.58 (d, J=8.7 Hz, 2H), 7.32 (bs, 2H), 7.23 (d, J=8.4 Hz, 1H), 6.97 (d, J=8.4 Hz, 2H), 4.79 (d, J=2.1 Hz, 2H), 3.59-3.55 (m, 1H), 2.53 (s, 3H); LCMS: purity: 97percent; MS (m/e): 428 (MH+).

The synthetic route of 6973-09-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rigel Pharmaceuticals, Inc.; Magilavy, Daniel; US2014/73659; (2014); A1;,
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These common heterocyclic compound, 34813-49-5, name is 2-Methylpropane-2-sulfonamide, 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. Product Details of 34813-49-5

General procedure: Inside a N2 filled glovebox, benzenesulfonamide (250 mg, 1.590 mmol) and copper(I) iodide (15.14 mg, 0.080 mmol), 4-toluene bromide (326mg, 1.91 mmol), potassium carbonate (550 mg, 3.98 mmol), Acetonitrile (4 mL), and N1,N2dimethylethane-1,2-diamine (70.1 mg, 0.795 mmol) was charged into a vial. The vial was then heated to 70 oC for 8hr, LC indicated >97% conversion of benzenesulfonamide. The reaction mixture was then cooled to room temperature. 2N HCl (4mL) was added slowly, followed by EtOAc extraction (5mL x 3). The organic layers were combined, concentrated, and flash chromatographed (SiO2, 20:1–> 3:1 Heptane:EtOAc) to give N(p-tolyl) benzene sulfonamide as white solids (380 mg, 97%).

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

Reference:
Article; Wang, Xiang; Guram, Anil; Ronk, Michael; Milne, Jacqueline E.; Tedrow, Jason S.; Faul, Margaret M.; Tetrahedron Letters; vol. 53; 1; (2012); p. 7 – 10;,
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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. 7700-07-4, name is N,N-Dimethylethenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of N,N-Dimethylethenesulfonamide

General procedure: A dried 25 ml, screw-sealed tube was charged with degassed [1,4 dioxane/water, 3 ml, 99:1 (v/v)], followed by the addition of 6 (140 mg, 1 mmol) and 3-chlorophenylboronic acid (624 mg, 4 mmol). After addition of [RhOH(cod)]2 (2 mol %, 9.1 mg, 0.02 mol) and rac-BINAP (6 mol %, 37 mg, 0.06 mol), the tube was closed. After removing air by vacuum the tube was back-filled with nitrogen and heated in a pre-heated oil bath at 120 C for 18 h. After cooling to room temperature, the resulting mixture was diluted with EtOAc (5 ml) and extracted with 5% aqueous NaHCO3 solution (5 ml). The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude obtained 7 was further purified by flash chromatography [silica gel 60 (0.040-0.063 nm, Merck)] eluent, Et2O-petroleum ether (40-60), 3:1 (v/v) or CH2Cl2 – EtOAc,, 95:5 (v/v), to give 158 mg of pure 7 (64%).

The synthetic route of 7700-07-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zilaout, Hicham; Van Den Hoogenband, Adri; De Vries, Jelle; Lange, Jos H.M.; Terpstra, Jan Willem; Tetrahedron Letters; vol. 52; 45; (2011); p. 5934 – 5939;,
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Adding a certain compound to certain chemical reactions, such as: 1444-94-6, name is 1,2-Cyclohexanedicarboximide, 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 1444-94-6, Application In Synthesis of 1,2-Cyclohexanedicarboximide

General procedure: To a suspension of corresponding cyclic imide 1a-1k (4mmol), potassium carbonate (4.4mmol) in DMF (5mL), 1-bromo-4-chlorobutane (1,2-dibromoethane (5 eq) for 2l, 1-bromo-3-chloropropane for 2m, 1-bromo-5-chloropentane for 2n) (4.4mmol) was added dropwise at 0C. The mixture was stirred at room temperature overnight and then partitioned between ethyl acetate (EA, 20mL) and water (30mL). The organic layer was washed successively with water (3¡Á30mL), saturated brine, and dried over anhydrous Na2SO4. The solvent was evaporated under vacuum and the residue was purified by column chromatography using petroleum ether(PE): EA (8:1) as eluent to give 2a-2n.

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, 1,2-Cyclohexanedicarboximide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Xu, Mingshuo; Wang, Yu; Yang, Feipu; Wu, Chunhui; Wang, Zhen; Ye, Bin; Jiang, Xiangrui; Zhao, Qingjie; Li, Jianfeng; Liu, Yongjian; Zhang, Junchi; Tian, Guanghui; He, Yang; Shen, Jingshan; Jiang, Hualiang; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 74 – 85;,
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Application of 3144-09-0, 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. 3144-09-0, name is Methylsulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Embodiment 80Under 80 C , the methanesulfonamide (0.75mmol, 71.3 mg) and (E) – 1,3-diphenyl-2-propen-1-ol (0.5mmol, 105.0 mg) and [BsTdmim]OTf (10mol %, 27.5 mg), 1,4-dioxane 2.0 ml is placed in a dry reaction flask, magnetic stirring reaction for 2h. After the completion of the reaction separation was done using column chromatography (by silica gel column, eluent: petroleum ether/ethyl acetate = 5/1), to obtain white solid (E)-N-(1,3-diphenylallyl)methanesulfonamide 142.1 mg, yield is 99%

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

Reference:
Patent; Lanzhou Institute of Chemical Physics; Xia, Chungu; Han, Feng; Wang, Lei; Li, Zhen; (27 pag.)CN103073372; (2016); B;,
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Electric Literature of 27466-83-7, 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. 27466-83-7, name is 4-Bromo-N-methylbenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Intermediate Preparation 154′-(2-(S)-Pyrrolidin-ylmethyl-pyrrolidine-1-carbonyl)-biphenyl-4-carboxylic acid methylamide Procedure Z’: To a stirring solution of 4-bromophenylmethyl amide (11.0 mmol, CAS No. 27466-83-7), bis-(pinacolato)diboron (1.1 mmol) and potassium acetate (3.0 mmol) in dimethyl sulfoxide (0.10M), add palladium(II) dichloride (dppf) complex with dichloromethane (1:1) (0.08 mmol). Heat reaction to 100 C. for 1.5 hours. After this time, cool the reaction to room temperature and add (4-bromo-phenyl)-(2-(S)-pyrrolidin-1-ylmethyl-pyrrolidin-yl)methanone (the product from preparation 14) (1.0 mmol), 2M aqueous sodium carbonate (3.0 mmol) add palladium(II) chloride (dppf) complex with dichloromethane (1:1) (0.08 mmol). Heat reaction to 100 C. for 18 hours. After this time, remove the heat and wash the reaction with water while extracting with 10% isopropanol/dichloromethane. Dry the organics with sodium sulfate, filter and concentrate in vacuo. Purify the title compound via radial chromatography eluting with 2M ammonia in methanol and dichloromethane. MS (m/e): 392.3 (M+1)

The synthetic route of 4-Bromo-N-methylbenzamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beavers, Lisa Selsam; Finley, Don Richard; Finn, Terry Patrick; Gadski, Robert Alan; Hipskind, Philip Arthur; Hornback, Wiliam Joseph; Jesudason, Cynthia Darshini; Pickard, Richard Todd; Takakuwa, Takako; Vaught, Grant Mathews; US2010/48580; (2010); A1;,
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Reference of 25900-61-2, 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. 25900-61-2, name is 3-Amino-N-methylbenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 9; N-(2-Diethylamino-ethyl)-4-(3-indan-5-yl-3H-[1 ,2,3]triazolo[4,5-d]- pyrimidin-5-ylamino)-benzamide (7); To a solution of 2,4-dichloro-5-nitropyrimidine (25.0 mg, 0.13 mmol) in THF (0.2 mL) was added a solution of 3-amino-N-methyl-benzamide (19.5 mg, 0.13 mmol) in isopropyl alcohol (0.5 mL)/dimethylformarnide (0.3 mL), and CsHCO3 (25.2 mg, 0.13 mmol) in water (0.016 mL total volume). The mixture was stirred at rt for 1.5 hr at which time 4-amino-N-(2-diethylamino-ethyl)-benzamideEtaCl (procainamide hydrochloride) (38.9 mg, 0.14 mmol) in isopropyl alcohol (0.5 mL)/dimethylformamide (0.3 mL) was added. The mixture was stirred at 50C for 20 hr, cooled to rt, and acetic acid (0.1 mL) was added. To the resulting slurry was added Zn dust (45 mg, 0.69 mmol); after stirring for 15 min at rt, the reaction solution was loaded onto a 1 g silica gel SPE cartridge and eluted with 6 mL of MeOH. The eluent was concentrated at reduced pressure, dried at approximately 1 mm Hg for 18 hr, and re-suspended in MeOH (1.0 mL). To this slurry was added HOAc (0.05 mL) and sodium nitrite (0.09 g, 1.3 mmol) in water (total volume 0.2 mL). The mixture was stirred at rt for 11 hr, loaded onto a 1 g C-18 SPE cartridge, and eluted with 6 mL of MeOH. The eluent was concentrated and the resulting residue was purified by reverse-phase liquid chromatography using a gradient of 90:10 (water:acetonitrile, with 0.1% TFA) to 10:90 (wateracetonitrile, with 0.1% TFA) to furnish (7) (0.0128 g, 0.018 mmol) as the bis TFA salt. HRMS (ES-TOF) calcd. for C25H30N9O2 m/z 488.2522 (M+H),+ found: 488.2514

The synthetic route of 3-Amino-N-methylbenzamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2006/76442; (2006); A2;,
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