Tag: M.W=100-200

Some common heterocyclic compound, 108-13-4, name is Malonamide, molecular formula is C3H6N2O2, 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 108-13-4

General procedure: An example of the preparation of the amide intermediate was carried out. Blocking the reaction vessel (when the amide intermediate is at a boiling point under normal pressure, etc.At or below the reaction temperature TB below) or to keep the reactor open (when the boiling point of the amide intermediate at normal pressure is higher than the reaction temperature TB described below), stirring is continued (600 r / min), The reaction temperature is changed to TB, and after maintaining the reaction temperature TB for TD hours, the reaction vessel is closed and connected to a vacuum pump, so that the degree of vacuum in the reaction vessel reaches 20-50 mbar (adjusted according to the type of nitrile product) to distill off As a nitrile product. The yield of the nitrile product was calculated and sampled for nuclear magnetic resonance spectroscopy and elemental analysis to characterize the obtained nitrile product. The specific reaction conditions and characterization results are shown in Tables A-6, A-7, A-8, A-9 and A-10 below. These characterization results indicate that the obtained nitrile product has an extremely high purity (99% or more).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108-13-4, its application will become more common.

Reference:
Patent; Sinopec Yangzi Petrochemical Co., Ltd.; Sinopec Corporation; Sun Hailong; Gao Yilong; Wei Yanyu; Chen Xinhua; Miao Jun; Li Na; Kan Lin; Bai Jiye; Chen Shaohui; Yang Aiwu; Xu Yuexing; (32 pag.)CN105016941; (2018); B;,
Amide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 104863-65-2, name is N-Methoxy-N-methylpropionamide, 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 104863-65-2, name: N-Methoxy-N-methylpropionamide

The reaction formula of this embodiment is as follows:In a 25 ml reaction flask, add compound 1a (0.3 mmol, 0.1561 g), compound 2i (15 mmol, 1.7573 g), water (30 muL), DCM (5 mL) to dissolve the above materials, and stir the reaction at 60 C. The reaction time is 3 h. After the reaction was completed, the solvent was removed by spin-drying, and the residue was subjected to flash column chromatography (PE: EA = 20: 1) to obtain pure product 3ai (0.0534 g) with a yield of 76%.

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-methylpropionamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Xuzhou Medical University; Wu Nan; Xu Zhou; Mi Jiajia; Li Chuang; Yuan Changyong; Zheng Yan; (15 pag.)CN110668937; (2020); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 91893-69-5, A common heterocyclic compound, 91893-69-5, name is 2-Amino-N,N-dimethylethanesulfonamide hydrochloride, molecular formula is C4H13ClN2O2S, 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: General procedure C: A mixture of amine hydrochloride (1.73 mmol), NaOH (0.10 g, 2.59 mmol) and ethanol (50 mL) was stirred and heated to reflux for 1 h. Then gossypol acetic acid (0.50 g, 0.86 mmol) was added and the reaction liquid continued to reflux for 5 h. The reaction mixture was cooled to room temperature and then the resulting solid was filtered, washed with ethanol and then recrystallized with pyridine and ethanol or chloroform and ethanol to give the desired gossypol derivatives. Data for 19: General procedure C; yellow solids; yield, 61.0%; mp, 235-237C; 1H NMR (400MHz, CDCl3) delta 13.47-13.37 (m, 2H), 9.64 (d, J=12.2Hz, 2H), 7.89 (s, 2H), 7.59 (s, 2H), 5.61 (s, 2H), 3.95 (dd, J=11.8, 6.5Hz, 4H), 3.76-3.66 (m, 2H), 3.26 (t, J=6.5Hz, 4H), 2.88 (s, 12H), 2.11 (s, 6H), 1.55-1.50 (m, 12H); 13C NMR (100MHz, CDCl3) delta 173.51, 162.80, 149.02, 146.96, 132.25, 129.22, 128.09, 118.37, 115.97, 114.40, 103.70, 48.57, 45.17, 37.28, 27.45, 20.34, 20.29, 20.07; HRMS (ESI) calcd for C38H49N4O10S2 (M-H)- 785.2896, found 785.2873.

The synthetic route of 91893-69-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Ling; Li, Zheng; Wang, Kailiang; Liu, Yuxiu; Li, Yongqiang; Wang, Qingmin; Bioorganic and Medicinal Chemistry; vol. 24; 3; (2016); p. 474 – 483;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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).

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; 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;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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;,
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. 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;,
Amide – Wikipedia,
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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;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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;,
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 758-96-3 as follows. Computed Properties of C5H11NO

Weigh benzothiazole (0.5mmol, 67mg), K2S2O8 (2mmol, 0.54g) and Eosin Y (0.01mmol, 6.5mg) in a 25mL Schlenk reaction tube, and then add N, N-dimethylpropionamide (38mmol, 3.8g), placed under a 20W LED white light to react, stirred the reaction at room temperature, followed by TLC to monitor the progress of the reaction, the reaction was completed after 24 hours, the reaction solution was concentrated to remove the solvent, and the concentrated solution was separated by column chromatography (eluent Petroleum ether / ethyl acetate) in a volume ratio of 5: 1) to give a yellow oil, the derivative Ik. The yield was 66%.

According to the analysis of related databases, 758-96-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Zhejiang University of Technology; Weng Jianquan; Xu Wenxiu; Dai Xiaoqiang; Liu Xinghai; (11 pag.)CN110432282; (2019); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 1882-71-9, name is 2-Amino-5-methoxybenzamide, 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 1882-71-9

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¡ãC. 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¡Á5mL) and acetone (2¡Á5mL), 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 2-Amino-5-methoxybenzamide 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;,
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Amide – an overview | ScienceDirect Topics