Category: amides-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 1015-89-0, name is Phenanthridin-6(5H)-one, 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 1015-89-0, Computed Properties of C13H9NO

Step 1: Synthesis of 2-bromophenanthridone 99.8 g (511 mmol) was added to the phenanthridine dinon 3 ? flask equipped with a plurality of necked stirring arm and is equipped with a condenser. It was added to 1.2 ? of glacial acetic acid and the mixture was stirred at 150 rpm, heated to reflux. A 90 g (562 mmol) Br2 dispersed in 100 acetic acid was added dropwise over 3 hours to a solution being refluxed. After the addition, the mixture was found to be analyzed is about 80% complete. Based on this analysis, it was added dropwise while refluxing the (in the 30 acid) Add 20 g of Br2 in the mixture. After the addition, the analysis is> 90% completed. It was added dropwise to 20 g Br2 end (30 of the acid) and the mixture was stirred for 1 hour after addition. Final analysis> was 97%. The mixture was cooled, water was added in 1 ?, and the mixture was filtered. By stirring in a wet solids aqueous solution of sodium thiosulfate was decomposed the residual bromine, and filtered again. thisRinse the solid with H2O, and allowed to dry under vacuum to remove residual water. Thereafter, the solid was recrystallized from nitrobenzene (> ? 2), and collected on a funnel to give 128 g of 2-bromo-phenanthridine dinon (90.8% yield).

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Reference:
Patent; UNIVERSAL DISPLAY CORPORATION; NOLIS, DAVID B; LIN, CHOOK; MCKINSEY, PETER BODON; CHAI, CHUI LEE; WALTERS, ROBERT W; PIERS, SCOTT A; BROWN, CORY S; IGOR, WALTER H; (101 pag.)KR2016/30582; (2016); A;,
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224789-21-3, name is 2-(2-Ethoxyphenyl)-5-methyl-7-propylimidazo[5,1-f][1,2,4]triazin-4(3H)-one, 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. Safety of 2-(2-Ethoxyphenyl)-5-methyl-7-propylimidazo[5,1-f][1,2,4]triazin-4(3H)-one

EXAMPLE 1 (procedure for the preparation of 4-ethoxy-3-(5-methyl-4-oxo-7-propyl-3,4- dihydroimidazo-[5,l-fJ[l,2,4]triazin-2-yl)benzenesulfonylchloride)A solution of 50 g of 2-(2-ethoxyphenyl)-5-methyl-7-propyl-3H-imidazo[5, l-f][l,2,4]triazin- 4-one, dissolved in 500 ml of dichloromethane was added dropwise to a solution of 100 ml of chlorosulfonic acid and 50 ml of dichloromethane during ca. 90 minutes. The mixture was further stirred at laboratory temperature (23 C) overnight, 24 hours in total. On the following day, the reaction mixture was poured into 800 g of ice. After the ice has thawed, the mixture was thoroughly mixed. The precipitated solid substance was filtered off, the filtration cake was washed with dichloromethane (2 x 100 ml) and the isolated solid product was vacuum dried (20 C, 1 to 2 kPa (10 to 20 mbar)). The product was obtained in the form of an off-white powder in the yields of from 1 10 to 1 15% (calculated on the non-protonated form of the product).

The synthetic route of 224789-21-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ZENTIVA, K.S.; HALAMA, Ales; STRELEC, Ivo; DAMMER, Ondrej; WO2013/75680; (2013); A1;,
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Application of 5004-88-6,Some common heterocyclic compound, 5004-88-6, name is 2-Amino-4,5-dimethoxybenzamide, molecular formula is C9H12N2O3, 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 mixture of 2-chlorobenzoic acid (1b) (0.61 g, 3.92 mmol) and thionyl chloride (1 mL) was heated for 2 h. The excess of thionyl chloride was recovered under reduced pressure and the residue so obtained was dissolved in dry dioxane (1 mL). The solution was then dropwise added to mixture of 2-amino-4,5-dimethoxybenzamide (2) (0.7 g, 3.57 mmol) and TEA (1.2 mL, 8.92 mmol) in dry dioxane (2 mL) at 10 C. The reaction mixture was stirred at rt for another 1 h and quenched into cold water (50 mL). The precipitate formed was filtered, washed with water and dried to obtain compound 3b (0.85 g, 71%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Amino-4,5-dimethoxybenzamide, its application will become more common.

Reference:
Article; Yadav, Mange R.; Grande, Fedora; Chouhan, Bishram S.; Naik, Prashant P.; Giridhar, Rajani; Garofalo, Antonio; Neamati, Nouri; European Journal of Medicinal Chemistry; vol. 48; (2012); p. 231 – 243;,
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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 164332-88-1 as follows. Quality Control of tert-Butyl (2-(2-bromoethoxy)ethyl)carbamate

Example 5-3-1 Preparation of tert-butyl (2-{2-[{5-(2-{2-[(tert- butoxycarbonyl)amino]ethoxy}ethoxy)-2-[1 -(4-ethoxy-2,6-difluorobenzyl)-1 H-indazol-3- yl]pyrimidin-4-yl}(pyridi -4-yl)amino]ethoxy}ethyl)carbamate35 mg 2-[1 -(4-ethoxy-2,6-difluorobenzyl)-1 H-indazol-3-yl]-4-(pyridin-4-ylamino)- pyrimidin-5-ol 5-1-1 (0.074 mmol, 1.0 eq.) was dissolved in 0.6 mL DMF. 31 mg potassium carbonate (0.22 mmol, 3.0 eq.) and 20 mg tert-butyl [2-(2- bromoethoxy)ethyl]carbamate 5-2-1 (0.074 mmol, 1 .0 eq.) were added. The reaction mixture was stirred at room temperature over night. 20 mg tert-butyl [2-(2- bromoethoxy)ethyl]carbamate 5-2-1 (0.074 mmol, 1 .0 eq.) was added and the reaction mixture was stirred for 2.5 h at room temperature. Butanone was added and the organic layer was washed with brine. The aqueous layer was extracted with butanone. The combined organic layers were dried with a waterresitent filter and concentrated in vacuo. The crude product was purified by flash chromatography to provide the 85% pure target compound: 20 mg, 0.03 mmol, 34%.retention time: 1 .20 minMS ES+: 662.3 [M+H]+

According to the analysis of related databases, 164332-88-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; MENGEL, Anne; LERCHEN, Hans-Georg; MUeLLER, Thomas; BAeRFACKER, Lars; HITCHCOCK, Marion; CLEVE, Arwed; BRIEM, Hans; SIEMEISTER, Gerhard; BONE, Wilhelm; FERNANDEZ-MONTALVAN, Amaury Ernesto; SCHROeDER, Jens; MOeNNING, Ursula; HOLTON, Simon; (224 pag.)WO2016/42080; (2016); A1;,
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Electric Literature of 6292-59-7, These common heterocyclic compound, 6292-59-7, name is 4-(tert-Butyl)benzenesulfonamide, 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 5-(2-methoxyphenoxy)-2-(2′-pyrimidinyl)-4,6-dihydroxy pyrimidine compound of formula-4 (100 g), POCI3 (500 ml) was added. Heated the reaction mixture to 90¡ãC and stirred for 30 min. The temperature of the reaction mixture was raised to 105¡ãC and was stirred for 8 hrs. The reaction mixture was cooled to 6O0C and concentrated to obtain a residue. The reaction mixture was quenched with ice water and toluene (1200 ml) was added to it. The pH was adjusted to 8-9 with 30percent sodium hydroxide solution. The organic and the aqueous layers were separated. The aqueous layer was extracted with toluene (200 ml). The organic layers were combined, washed with water and dried. The solvent was concentrated to 1200 ml and a solution of 4-tert- butyl benzene sulfonamide (6) (48 g) in toluene (600 ml), potassium carbonate (35 g) and tetra butyl ammonium bromide (10 g) was added and the reaction mixture was heated to 50¡ãC. The reaction mixture was heated to refluxed using dean stark apparatus for 10 hrs. The reaction mixture was cooled to 25¡ãC.The solid obtained was filtered and made slurry in water. The solid was filtered, washed with water and dried. Yield: 92 g

Statistics shows that 4-(tert-Butyl)benzenesulfonamide is playing an increasingly important role. we look forward to future research findings about 6292-59-7.

Reference:
Patent; MSN LABORATORIES LIMITED; WO2009/95933; (2009); A2;,
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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. 830-43-3, name is 4-(Trifluoromethyl)benzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 4-(Trifluoromethyl)benzenesulfonamide

General procedure: In 25ml RB flask to a solution of Compound 9 (200 mg) in dry DMF (5ml), EDCI (250 mg, 1.25eq) and DMAP (130 mg,1eq) were added followed by addition of Sulfonamide (1eq). RM was stirred at RT for 4hrs. Solvent from the reaction mixture was evaporated. To the residue water was added and acidified with 6N HCl, solid precipitated out. Solid was filtered and dried. Crude solid was purified by flash chromatography eluating with 4-8% MeOH/DCM as solvent system to give pure product.

The synthetic route of 830-43-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Patil, Vikas; Kale, Manoj; Raichurkar, Anandkumar; Bhaskar, Brahatheeswaran; Prahlad, Dwarakanath; Balganesh, Meenakshi; Nandan, Santosh; Shahul Hameed; Bioorganic and Medicinal Chemistry Letters; vol. 24; 9; (2014); p. 2222 – 2225;,
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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. 406233-31-6, name is 4-Fluoro-3-nitrobenzenesulfonamide, A new synthetic method of this compound is introduced below., name: 4-Fluoro-3-nitrobenzenesulfonamide

General procedure: To an ice cold stirred solution of compound 4a-4u (1 eq) in anhydrousDCM (10 mL for 1 mmol of substrate), TEA (3 eq) was added dropwise and stirred for 10 min. Compound 5 (1 eq) was added slowly andstirred at RT for 16 h (precipitation was observed during the reactionprogress). TLC showed completion of reaction. The reaction mixturewas concentrated under reduced pressure. Water was added to thecrude material and stirred for 30 min. Obtained solid was filtered,washed with water and dried under vacuum. The solid was trituratedwith ethyl acetate, filtered and dried under high vacuum to affordcompound 6a-v.

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; Kalisha Vali; Gundla, Rambabu; Singh, Om V.; Tamboli, Yasinalli; Di Cesare Manelli, Lorenzo; Ghelardini, Carla; Al-Tamimi, Abdul-Malek S.; Carta, Fabrizio; Angeli, Andrea; Supuran, Claudiu T.; Bioorganic Chemistry; vol. 92; (2019);,
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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. 3118-68-1, name is 3-Cyanobenzenesulfonamide, A new synthetic method of this compound is introduced below., category: amides-buliding-blocks

Production Example 27 N-hydroxy-3-sulfamoylbenzene carboximidamide A mixture of 3-cyanobenzenesulfonamide (5.00 g), 50% hydroxylamine aqueous solution (1.84 mL) and ethanol (27 mL) was heated to reflux for 6 hours. Thereafter, the reaction solution was concentrated under a reduced pressure, so as to obtain the title compound (5.80 g) in the form of a colorless amorphous substance. 1H NMR (600 MHz, DMSO-d6) delta ppm 5.92 (s, 2H) 7.36 (s, 2H) 7.57 (t, J=7.79 Hz, 1H) 7.72-7.93 (m, 2H) 8.09-8.21 (m, 1H) 9.80 (s, 1H); MS (ESI neg.) m/z: 214 [M-H]-

The synthetic route of 3118-68-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD.; Nakamura, Toshio; Sakagami, Kazunari; Konishi, Kazuhide; Yamamoto, Kanako; Masuda, Seiji; Matsuda, Yohei; Okada, Kumiko; Shibata, Tsuyoshi; Ohta, Hiroshi; Yasuhara, Akito; Kawamoto, Hiroshi; Amada, Hideaki; Urabe, Hiroki; Nishikawa, Rie; Kashiwa ASHIWA, Shuhei; US2013/137865; (2013); A1;,
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Related Products of 2603-10-3, 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 2603-10-3 as follows.

In a fixed bed reactor, 20 g of a supported heteropoly solid acid catalyst having a phosphomolybdic acid content of 1% added, the dimethyl carbonate was continuously added to a fixed bed reactor with a pump, and the temperature was raised to 80 C. Respectively, the preheating mass concentration of 5% phenylcarbamic acid methyl ester-dimethyl carbonate solution and concentration 10% formaldehyde solution to 80 C and simultaneously with a pump in a fixed bed reactor, Adjust the flow rate of phenylcarbamic acid methyl ester-dimethyl carbonate solution 0.4 ml/min, formaldehyde solution flow rate of 0.1 ml/min, Under normal pressure conditions for continuous condensation reaction, reaction material timing sampling analysis,MDC conversion rate of 99. 1%,The selectivity was 81.6%.Distillation crystallization gave dimethyl 4,4′-diphenylmethane dicarbamate.

According to the analysis of related databases, 2603-10-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; China Petroleum & Chemical Corporation; Research Institute of Nanjing Chemical Industry Group; He, yu miao; Jin, Hanjiang; Wu, Qijian; Jin, Yu Cun; Liu, Zhuo; Chen, Yongping; (5 pag.)CN106565545; (2017); A;,
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Electric Literature of 513-74-6, These common heterocyclic compound, 513-74-6, name is Ammonium carbamodithioate, 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: Following literature procedures,1 ammonia gas was bubbled into carbon disulfide 1 (16.7g, 0.22 mol) in THF (100 ml) keeping the temperature below 45 ¡ãC. After 1 hr, the reaction was stopped by allowing the temperature to decrease to rt. The excess ammonia gas was removed by streaming N2 for 30 min or by rotary evaporation under vacuum. The precipitate was collected by filtration to afford white solid ammonium dithiocarbamate 2 (23.1 g, 96percent). Methyl iodide (17.8 g, 0.125 mol) was added to a solution of 2 (5.5 g, 0.05 mol) in acetone (100 ml) at rt and the mixture was stirred for 24 hr. The solid was collected by filtration, washed with chilled acetone (20 ml) and dried under vacuum to provide white solid S,S?-dimethyliminodithiocarbonate hydroiodide ammonium iodide 3 (18.9 g, 96percent). 3 (7.9 g, 0.02 mol) was treated with sat. aq. NaHCO3 solution (100 ml x 2) and the organic products extracted with dichloromethane (50 ml). The organic layer was dried over Na2SO4 and concentrated in vacuo to a clear, colorless liquid 4 (2.3 g, 95percent). 1H NMR (400 MHz, CDCl3) delta 8.88 (s, 1H), 2.42 (s, 6H). 13C NMR (101 MHz, CDCl3) delta 172.10, 14.50. HRMS (ESI+) m/z calcd for C3H8N+ 122.0098, found 122.0096.

Statistics shows that Ammonium carbamodithioate is playing an increasingly important role. we look forward to future research findings about 513-74-6.

Reference:
Article; Pollock, Julie A.; Kim, Sung Hoon; Katzenellenbogen, John A.; Tetrahedron Letters; vol. 56; 44; (2015); p. 6097 – 6099;,
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