Amides-buliding-blocks

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. 90-16-4, name is Benzo[d][1,2,3]triazin-4(3H)-one, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H5N3O

A mixture of compound (20 g), obtained from step f of Example 1, triphenyl phosphine (17.6 g) and l,2,3-benzotriazin-4(3H)-one (7.2 g) were dried in high vacuum in a round bottom flask for 10 minutes. The vacuum was released under a nitrogen atmosphere and tetrahydrofuran (200 mL) was added to the above reaction mixture. The reaction mixture was cooled to O0C and diisopropyl azodicarboxylate (9.8 mL) was added slowly. The reaction mixture was stirred for 30 minutes at same temperature, and then quenched with water and extracted with ethyl acetate. The organic layer was washed with water, brine solution, dried over anhydrous sodium sulphate and concentrated to obtain a residue which was purified by column chromatography over silica gel using 30% ethylacetate in hexane as eluant to afford the title compound (22 g). Mass (m/z): 586.24 (M+ +1).

According to the analysis of related databases, 90-16-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; RANBAXY LABORATORIES LIMITED; WO2008/23336; (2008); A2;,
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Some common heterocyclic compound, 123986-64-1, name is tert-Butyl 4-(hydroxymethyl)benzylcarbamate, molecular formula is C13H19NO3, 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. Formula: C13H19NO3

3) Synthesis of 1-[4-[N-(tert-butoxycarbonyl)aminomethyl]benzyl]-4-phenylpiperidine To a solution of 5.0 g (21.07 mM) of 4-[N-(tert-butoxycarbonyl)aminomethyl]-1-phenylmethanol and 5.9 ml (42.33 mM) of triethylamine in THF (42 ml) was added 2.5 ml (32.3 mM) of methanesulfonyl chloride at 0 C. and the mixture was stirred at the prevailing temperature for one hour. The reaction was then stopped by adding saturated aqueous solution of sodium hydrogen carbonate and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous solution of sodium chloride and dried over MgSO4. The solvent was then distilled off under reduced pressure to provide 6.72 g (21.07 mM) of crude product as light-brown solid. To a solution of 6.72 g (21.07 mM) of this crude mesylate in ethanol (42 ml) was added 5.9 ml (42.33 mM) of triethylamine as well as 3.40 g (21.09 mM) of 4-phenylpiperidine and the mixture was refluxed for 18 hours. After cooling to room temperature, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After concentration, the crude product was purified by column chromatography (ethyl acetate-hexane: 50%) to provide the title compound as light-yellow solid. Yield 5.77 g (72%) m.p. 73-74 C. 1H-NMR (200 MHz, CDCl3) delta: 1.46 (9H, s), 1.73-1.88 (4H, m), 1.99-2.19 (1H, m), 2.94-3.08 (2H, m), 3.54 (2H, s), 4.31 (2H, d, J=5.8 Hz), 4.73-4.96 (1H, m), 7.13-7.36 (4H, m). IR (KBr): 3389, 1690, 1518, 1269, 1171 cm-1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 123986-64-1, its application will become more common.

Reference:
Patent; Takeda Chemical Industries, Ltd.; US6235731; (2001); B1;,
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Reference of 1129-26-6,Some common heterocyclic compound, 1129-26-6, name is 4-Methoxybenzenesulfonamide, molecular formula is C7H9NO3S, 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 the intermediates compound2a-2d (1 mmol) with triethylamine (2 mmol) into DMF(12 mL), then a mixture of 1-ethyl-(3-(3-dimethylamino)-propyl)-carbodiimide hydrochloride (EDCI) (1 mmol) andN-hydroxybenzotriazole (HOBt) (1 mmol) was placed in thereaction system, stirred at room temperature for 30 min, themixture of substituted benzene sulfonamide (1 mmol) andDMF (5 mL) was added in the reaction system, the reactionmixture was monitored by TLC. After completion of the reaction,the product was extracted from chloroform with water,0.2 mol/L hydrochloric acid, water, 2.0 mol/L sodium hydroxide,saturated sodium chloride successively, and then dried,concentrated, and purified by preparative thin layer chromatographyfollowed by recrystallization from ethanol.

The synthetic route of 1129-26-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lv, Xian-Hai; Ren, Zi-Li; Liu, Hao; Li, Hai-Dong; Li, Qing-Shan; Wang, Li; Zhang, Li-Song; Yao, Xiao-Kang; Cao, Hai-Qun; Chemical and Pharmaceutical Bulletin; vol. 66; 4; (2018); p. 358 – 362;,
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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. 915087-25-1, name is 4-Amino-2-fluoro-N-methylbenzamide, A new synthetic method of this compound is introduced below., category: amides-buliding-blocks

Example 3: Preparation of formula 4 TMSCN [74 g] was combined with N-methyl-2-fluro-4-aminobenzamide [formula 3, 50 g] in a clean and dried RBF. Acetic acid [250 ml] was slowly added dropwise to create frothing. Next, acetone [250 ml] was added and the reaction mass was heated to about 85 C. Heating continued until the reaction was complete. Next, the solvents were completely distilled off under vacuum (680 + 30 mm Hg). The resultant solid residue was cooled to room temperature, water [1000 ml] was added to the residue, and the reaction mass was stirred to get a free-flowing solid. The solid was filtered and washed with water to form a slurry. The slurry was then washed with tert-butyl methyl ether (TBME). The filtered cake was suck dried and the product dried under vacuum to result in formula 4.

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; MYLAN LABORATORIES LTD; WAGH, Ghanshyam; BODUPALLI, Murali; YEWALE, Sampat; DHANANJAY, Shinde; GADAKAR, Mahesh Kumar; GORE, Vinayak; DANDALA, Ramesh; (19 pag.)WO2016/38560; (2016); 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. 24036-52-0, name is 6-Bromo-2H-1,4-benzoxazin-3(4H)-one, A new synthetic method of this compound is introduced below., COA of Formula: C8H6BrNO2

A mixture of 6-bromo-2H-benzo[b][1,4]oxazin-3(4H)-one (197 mg, 0.864 mmol), (S)-3-phenylmorpholine (172.7 mg, 1.058 mmol), 2-(dicylclohexylphosphino)-2′-(N,N-dimethylamino)biphenyl (11.2 mg, 0.028 mmol), tris(dibenzylideneacetone)dipalladium (0) (8.9 mg, 0.01 mmol), tetrahydrofuran (3.3 mL) and lithium bis(trimethylsilyl)amide in tetrahydrofuran (1 M, 1.93 mL, 2 mmol) was stirred at 70 C. overnight. The mixture was cooled to room temperature and saturated aqueous ammonium chloride and ethyl acetate were added. The layers were separated and the aqueous layer was extracted with ethyl acetate (3*). The organic layers were combined, dried over magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel column chromatography (gradient: 0-25% ethyl acetate in heptanes) to afford the title compound (105.6 mg, 39.4%). 1H NMR (400 MHz, CHLOROFORM-d) delta ppm 3.01(1H, ddd, J=12.2, 9.3, 4.3 Hz), 3.29 (1H, m), 3.54 (1H, dd, J=11.4, 8.9 Hz), 3.92 (3H, m), 4.15 (1H, m), 4.48 (2H, s), 5.28 (1H, s), 6.37 (1H, d, J=2.5 Hz), 6.56 (1H, m), 6.72 (1 H, d, J=8.8 Hz), 7.16 (3H, m), 7.26 (1H, m), 7.24 (2H, s), 7.97 (1H, s).

The synthetic route of 24036-52-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pfizer Inc; US2011/281854; (2011); A1;,
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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. 672-58-2, name is 3-(Trifluoromethyl)benzenesulfonamide, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H6F3NO2S

General procedure: To a stirred solution of glucal (1 equiv.) and N-nucleophile (1.1 equiv.) inanhydrous 1,2-dichloroethanne (2 mL/mmol) under an atmosphere of argon was added Zn(OTf)2 (10 mol%) at 40?C. The reaction mixture was stirred untilthe complete consumption of the starting material (glycal). The solvent wasfiltered and concentrated in vacuo, and the crude residue was redissolved indichloromethane and loaded on a silica gel column. The product was purified by silica gel column chromatography using hexane/EtOAc as the eluent to affordthe 2,3-unsaturated N-glycosides. All of the products were confirmed by1H NMR, 13C NMR, and MS/HRMS spectroscopy and compared with that of literature data; characterization data of new products are outlined in the experimentalsection

According to the analysis of related databases, 672-58-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Reddy, Thurpu Raghavender; Battina, Suresh Kumar; Kashyap, Sudhir; Journal of Carbohydrate Chemistry; vol. 34; 3; (2015); p. 133 – 144;,
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Related Products of 1891-90-3, A common heterocyclic compound, 1891-90-3, name is 4-(Trifluoromethyl)benzamide, molecular formula is C8H6F3NO, 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.

First access in the microchannel reactor15 minutes of nitrogen replacement system air,Under full nitrogen protection conditions,Cool down at -30~-25C and start to join.95.5 g (0.5 mol, 99%)P-trifluoromethylbenzamide and 500a mixture of milliliters of methyl tert-butyl ether,At the same time, 0.323 liter (0.55 mol, 1.7 mol/L) was added dropwise.Tert-butyl lithium solution,The reaction solution is all introduced into a cryogenic collector to obtain a compound (III);Compound (III) and 66.1 g (0.6 mol, 99%) were then metered with a metering pump.The methyl methanesulfonate is kept between -30 and -25 C.Finished through the microchannel reactor for 1.5 hours,After the addition, the sample analysis did not detect trifluoromethylbenzamide.The reaction solution is slowly added to the person under nitrogen protection conditions.In ice water between 0-5 C,The solvent is removed by distillation under reduced pressure to give a yellow solid;Nuclear magnetic confirmation as the target product2-Methylsulfonyl-4-trifluoromethylbenzamide.The amount is 132 grams,97.8%,The yield was 96.7%.

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; Papanna (Beijing) Technology Co., Ltd.; Xing Wenlong; Fu Renji; (7 pag.)CN109705005; (2019); A;,
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Electric Literature of 366-49-4, 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 366-49-4 as follows.

To a solution of N-(5-fluoro-2-methylphenyl)acetamide (XXV) (120 g, 717 mmol, 1.0 eq) in HOAc (3 L) was added a solution of Br2 (140 g, 876 mmol, 1.2 eq) in HOAc (1 L) dropwise. The mixture was stirred at 25 C for 3 h. LC/MS showed compound 2 was (XXV) completely consumed. The reaction mixture was quenched with water (8 L). The solid was filtered, washed with water and petroleum ether. The solid was dried in vacuo to give N-(4-bromo-5-fluoro- 2-methylphenyl)acetamide (XXVI) as a white solid (155 g, 629.9 mmol, 87.8% yield). NMR (CDC13, 400 MHz) delta ppm 2.20 (s, 6H), 7.07 (brs, 1H), 7.32 (d, J = 7.2 Hz, 1H), 7.85 (d, J = 10.8 Hz, 1H); ESIMS found C9H9BrFNO mlz 247.2 (M+l).

According to the analysis of related databases, 366-49-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SAMUMED, LLC.; KC, Sunil Kumar; WALLACE, David Mark; CAO, Jianguo; CHIRUTA, Chandramouli; HOOD, John; (265 pag.)WO2017/24010; (2017); 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. 402-46-0, name is 4-Fluorobenzenesulfonamide, A new synthetic method of this compound is introduced below., COA of Formula: C6H6FNO2S

100 mg of 4-fluorobenzensulfonamide (0.71 mmol) dissolved with allylamine (434 muL, 5.71 mmol) in a sealed tube was heated at 110 C for 14 days. Then, the mixture was cooled to room temperature and was diluted with MeOH. The solvent was evaporated and the crude mixture was purified by combi-flash with the eluent petroleum ether/ethylacetate: 70/30, thereby obtaining compound 7 (62 mg, 51%) as an orange solid (mp: 74-76 C). 1H NMR (CD3COCD3, 400 MHz, ppm) d: 3.85 (td, CH2, J = 5.5 Hz, J = 1.7 Hz, H10), 5.12 (ddt, 1H, J = 10.3 Hz, J = 1.6 Hz, J = 1.6 Hz, H3′), 5.26 (ddt, 1H, J = 17.2 Hz, J = 1.8 Hz, J = 1.8 Hz, H3′), 5.89 (broad s, 1H, NH), 5.93 (m, CH, H2′), 6.16 (s, SO2NH2), 6.69 (d, 2CH, J = 8.9 Hz, H3 and H5), 7.60 (d, 2CH, J = 8.9 Hz, H2 and H6). 13C NMR (CD3COCD3, 100 MHz, ppm) d: 46.1 (CH2, C1′), 112.2 (2CH, C3 and C5), 116.1 (CH2, C30), 128.7 (2CH, C2 and C6), 131.7 (C1), 136.1 (CH, C2′), 152.5 (C4). MS (IES+, ACN): m/z 213 [M+H]+. HRMS (ESI, CH3OH): m/z 235.0518 (m/z theoretical: 235.05172) [M+Na]+.

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:
Article; Compain, Guillaume; Martin-Mingot, Agnes; Maresca, Alfonso; Thibaudeau, Sebastien; Supuran, Claudiu T.; Bioorganic and Medicinal Chemistry; vol. 21; 6; (2013); p. 1555 – 1563;,
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Adding a certain compound to certain chemical reactions, such as: 54616-47-6, name is 2-Bromo-N,N-dimethylbenzamide, 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 54616-47-6, Recommanded Product: 54616-47-6

General procedure: To a stirred solution of 1 (0.23 g, 1.0 mmol) in THF (6 mL) at -78C was added n-BuLi (1.6 M in hexane; 1.0 mmol) dropwise. After 15 min, PhNCS(0.14 g, 1.0 mmol) was added and stirring was continued for an additional 5 min before addition of saturated aqueous NH4Cl (15 mL). The mixture was extracted with AcOEt (3 ¡Á 10 mL), and the combined extracts were washed with brine (10 mL), dried (Na2SO4) and concentrated by evaporation

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, 2-Bromo-N,N-dimethylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kobayashi, Kazuhiro; Shigemura, Yuuho; Fujiwara, Daiki; Heterocycles; vol. 94; 6; (2017); p. 1152 – 1158;,
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