Sources of common compounds: 86-86-2

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Adding a certain compound to certain chemical reactions, such as: 86-86-2, name is 1-Naphthaleneacetamide, 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 86-86-2, COA of Formula: C12H11NO

General procedure: A mixture of the amide (1, 1 mmol), alcohol (15 mL), and pulverized potassium bisulfate (1.1 g, 8 mmol) was refluxed for the specified time. The alcohol was removed in vacuo and the residue was triturated with hexanes (or other appropriate solvent such as DCM or ethyl acetate to dissolve the product). Removal of hexanes in vacuo provided the following pure products

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:
Article; Sattenapally, Narsimha; Sharma, Jhanvi; Hou, Yuqing; Arkivoc; vol. 2018; 5; (2018); p. 174 – 183;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Sources of common compounds: 89979-12-4

According to the analysis of related databases, 89979-12-4, the application of this compound in the production field has become more and more popular.

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. 89979-12-4, name is 5-Chloro-2-(methylsulfonamido)benzoic acid, This compound has unique chemical properties. The synthetic route is as follows., name: 5-Chloro-2-(methylsulfonamido)benzoic acid

Mixed 5-chloro-2-(methylsulfonamido)benzoic acid (28mg, 0.109mmol) with HATU (42mg, 0.109mmol) and dissolved in anhydrous DMF (300uL). Stirred for Ihr. Dissolved hydrogenation product in anhydrous DMF (300uL) and added to the reaction. Added TEA (30uL, 0.218mmol).Stirred for 12 hrs. Diluted with acetonitrile and purified with Prep HPLC to give compound 40 (22mg, 32% yield).1H NMR (400MHz, CD3OD): delta 7.49 (m, 3H), 6.26 (m, 1H), 6.08 (m, 1H), 4.78 (m, 1H), 4.57 (m, 2H), 4.14 (m, 2H), 3.47-3.34 (m, 2H), 3.01 (m, 4H), 2.76 (s, 3H), 2.40-2.05 (m, 2H), 1.73- 1.50 (m, 4H). LC/MS (m/z): 519.2 [M+H]+

According to the analysis of related databases, 89979-12-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GILEAD SCIENCES, INC.; BABAOGLU, Kerim; BOOJAMRA, Constantine, G.; EISENBERG, Eugene, J.; HUI, Hon Chung; MACKMAN, Richard, L.; PARRISH, Jay, P.; SANGI, Michael; SAUNDERS, Oliver, L.; SIEGEL, Dustin; SPERANDIO, David; YANG, Hai; WO2011/163518; (2011); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Continuously updated synthesis method about 5466-88-6

The synthetic route of 5466-88-6 has been constantly updated, and we look forward to future research findings.

Reference of 5466-88-6, A common heterocyclic compound, 5466-88-6, name is 2H-1,4-Benzoxazin-3(4H)-one, molecular formula is C8H7NO2, 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.

4-(4-Bromobutan-1-yl)-3,4-dihydro-2H-1,4-benzoxazin-3(4H)-one from 3,4-dihydro-2H-1,4-benzoxazin-3(4H)-one and 1,4-dibromobutane

The synthetic route of 5466-88-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; H. Lundbeck A/S; US2003/191133; (2003); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Analyzing the synthesis route of 402-46-0

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

These common heterocyclic compound, 402-46-0, name is 4-Fluorobenzenesulfonamide, 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. Quality Control of 4-Fluorobenzenesulfonamide

Example 44; 4-{2-[4-(4-Sulfamoylphcnyl)pipcrazin-l-yl]cthyl}pipcridinc-l-carboxylic acid tert-butyl ester hydrochloride; EPO A mixture of 4-fluorobenzenesulfonamide (1.00 g, 5.71 mmol) and piperazine (2.46 g, 28.54 mmol) in water (12 mL) was heated at 1000C for 2Oh. The resulting precipitate was collected filtration and washed with water and toluene to give 4-piperazin-l- ylbenzenesulfonamide: RT = 0.49 min; m/z (ES+) = 242.13 [M+H]+. A solution of 4-piperazin- 1-ylbenzenesulfonamide (0.46 g, 1.89 mmol) and 4-(2-oxoethyl)piperidine-l-carboxylic acid tert-butyl ester (0.43 g, 1.89 mmol) in DCM (50 mL) and THF (7 mL) with molecular sieves (0.90 g) was stirred under argon at rt for Ih. Sodium acetoxyborohydride (0.52 g, 2.46 mmol) was added and the reaction mixture was stirred for a further 2.5h. The reaction mixture was quenched with saturated NaHCO3 solution and extracted with EtOAc. The organic extracts were washed with brine, dried (MgSO4) and the solvent was removed under vacuum. The resulting solid was purified by recrystallisation (EtOAc) then dissolved in THF and 1 M HCl in dioxane (0.95 equivalents), the solvent was removed under vacuum and the resulting solid was washed with Et2O to afford the title compound: RT = 2.51 min; m/z (ES+) = 453.33 [M+H]+.

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

Reference:
Patent; PROSIDION LIMITED; WO2007/3964; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Simple exploration of 830-43-3

Statistics shows that 4-(Trifluoromethyl)benzenesulfonamide is playing an increasingly important role. we look forward to future research findings about 830-43-3.

Application of 830-43-3, These common heterocyclic compound, 830-43-3, name is 4-(Trifluoromethyl)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.

General procedure: Pyridine (5 mol) was added to a stirred solution of corresponding amine (1.0 mol) in THF (10 v), after 5 minutes, sulfonyl chloride derivative (1.1 mol) was added, stirred at room temperature under argon atmosphere for 16 h. Then the reaction mixture was diluted with water (50 v), extracted with EtOAc (50 v X 2), evaporated the solvent in vacuo, the crude product was purified by column chromatography to afford 8/9(a-c) and 12/13(a-b) (58-86%) as solids. During thesynthesis of N-(4-(3-((3S,4S)-3,4-Dihydroxypyrrolidin-1-yl)-3-oxopropyl)phenyl)-4-(trifluoromethyl)benzenesulfonamide (13b), isolated 29% of disulphonation product N-(4-(3 N-(4-(3-((3S,4S)-3,4-Dihydroxypyrrolidin-1-yl)-3-oxopropyl)phenyl)-4-(trifluoromethyl)-N-(4-(trifluoromethyl)phenylsulfonyl)benzenesulfonamide (13c) as white solid.

Statistics shows that 4-(Trifluoromethyl)benzenesulfonamide is playing an increasingly important role. we look forward to future research findings about 830-43-3.

Reference:
Article; Kasturi, Sivaprasad; Surarapu, Sujatha; Uppalanchi, Srinivas; Anireddy, Jaya Shree; Dwivedi, Shubham; Anantaraju, Hasitha Shilpa; Perumal, Yogeeswari; Sigalapalli, Dilep Kumar; Babu, Bathini Nagendra; Ethiraj, Krishna S.; Bioorganic and Medicinal Chemistry Letters; vol. 27; 12; (2017); p. 2818 – 2823;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

The origin of a common compound about 128263-66-1

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route N-(4-(Aminomethyl)phenyl)methanesulfonamide hydrochloride, its application will become more common.

Application of 128263-66-1,Some common heterocyclic compound, 128263-66-1, name is N-(4-(Aminomethyl)phenyl)methanesulfonamide hydrochloride, molecular formula is C8H13ClN2O2S, 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.

Example I N-[4-[[2-Hydroxy-3-(3-methylphenoxy)propyl]aminomethyl]phenyl]methanesulfonamide hydrochloride Heat a mixture of N-[4-(aminomethyl)phenyl]methanesulfonamide hydrochloride(15.0 g, 63.4 mmol) and 1,2-epoxy-3-phenoxypropane (10.41 g, 63.4 mmol) in 63.4 mL of 1 N KOH in methanol and 10 mL of water for about 3.5 h. Remove the solvent to afford crystals of the title compound. NMR (DMSO-d6): delta=2.27(s,3), 2.85-3.15(m,2), 3.02 (s,3), 3.93(s,2), 4.14(s,2), 4.23(br s,1), 5.90(br s,1), 6.74(m,3), 7.19(m,1), 7.24(d,2), 7.53(d,2), ca. 9.35 (br s,2) and 9.97(s,1) ppm.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route N-(4-(Aminomethyl)phenyl)methanesulfonamide hydrochloride, its application will become more common.

Reference:
Patent; Schering AG; US5051423; (1991); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Introduction of a new synthetic route about 6228-73-5

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

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 solution of 207.2 (0.270g, 0.79mmol, l .Oeq) in 1,4-dioxane (3mL) was added cyclopropane carboxamide (O. lOlg, 1.19mmol, 1.5eq), potassium carbonate (0.27g, 1.98mmol, 2.5eq). The reaction mixture was degassed for 10 min. under argon atmosphere, then tris(dibenzylideneacetone)dipalladium(0) (0.072g, 0.079mmol, O. leq) and 4,5-Bis(diphenylphosphino)-9,9-dimethylxanthene (0.091g, 0.158mmol, 0.2eq) were added, again degassed for 5 min. The reaction was stirred at 130C for 2h under microwave irradiation. After completion of reaction, reaction mixture was cooled to room temperature, transferred in water and product was extracted with ethyl acetate. Organic layer was combined, washed with brine solution, dried over sodium sulphate and concentrated under reduced pressure to obtain crude material. This was further purified by column chromatography using 2% methanol in dichloromethane as eluant to obtain pure 207.3 (0.250g, 81.03%). MS(ES): m/z 390.25 [M+H]+

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

Reference:
Patent; NIMBUS LAKSHMI, INC.; GREENWOOD, Jeremy Robert; HARRIMAN, Geraldine C.; LEIT DE MORADEI, Silvana Marcel; MASSE, Craig E.; MCLEAN, Thomas H.; MONDAL, Sayan; (401 pag.)WO2018/71794; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Extended knowledge of 630-22-8

The synthetic route of 630-22-8 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 630-22-8,Some common heterocyclic compound, 630-22-8, name is 2,2-Dimethylpropanethioamide, molecular formula is C5H11NS, 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 2-propen-1 -yl {3-[(2-chloro-4-pyrimidinyl)acetyl]-2- fluorophenyl}carbamate (30 g, 85.9 mmol) in DMA (300 ml_), NBS (15.3 g, 85.9 mmol) was added. The reaction mixture was stirred at room temperature for 1 h. Then 2,2-dimethylpropanethioamide (1 1 .0 g, 94.5 mmol) was added at 0 C. The mixture was stirred at room temperature for 2 h. The mixture was poured into water and extracted with EtOAc (200 ml_ x 3). The combined organic layers were washed with water and brine successively, dried over Na2SO , filtered and concentrated under reduced pressure to give the crude product, which was purified by column chromatography on silica gel(DCM etroleum ether 2:1 ) to afford the title compound. 1 1 g (35.4 % yield) 1 H NMR (400 MHz, CDCI3) delta ppm 8.29 (d, J=5.27 Hz, 1 H), 8.12-8.19 (m, 1 H), 7.12-7.25 (m, 2H), 6.80-6.88 (m, 2H), 5.85-5.98 (m, 1 H), 5.20-5.37 (m, 2H), 4.61 -4.67 (m, 2H). MS (ES+): 447 [M+H]+ .

The synthetic route of 630-22-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE LLC; ADAMS, Jerry, Leroy; FAITG, Thomas; KASPAREC, Jiri; PENG, Xin; RALPH, Jeffrey; RHEAULT, Tara Renae; WATERSON, Alex Gregory; WO2011/59610; (2011); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Introduction of a new synthetic route about 402-46-0

The synthetic route of 402-46-0 has been constantly updated, and we look forward to future research findings.

402-46-0, name is 4-Fluorobenzenesulfonamide, 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. Formula: C6H6FNO2S

Synthesis Example 6 Synthesis of N-(4-fluorophenylsulfonyl)-2-chloro-6-methoxyisonicotinamide (Compound No. 38) 1.75 g (0.01 mol) of 4-fluorobenzenesulfonamide were dissolved in 30 ml of pyridine, and added dropwise by 2.06 g (0.01 mol) of 2-chloro-6-methoxyisonicotinoyl chloride at 0 C. to 5 C., followed by agitation for 2 hrs. at room temperature. After acidified by adding aqueous hydrochloric acid, the precipitate was extracted by ethyl acetate. The organic layer obtained was dried and them concentrated to precipitate crude crystals, which were recrystallized by n-hexane/ethylacetate to 2.1 g (yield: 61.0%) of N-(4-fluorophenylsulfonyl)-2-chloro-6-methoxy isonicotinamide as white crystal.

The synthetic route of 402-46-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nippon Kayaku Kabushiki Kaisha; US4690934; (1987); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Simple exploration of 195986-74-4

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.

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. 195986-74-4, name is 7-Bromo-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione, A new synthetic method of this compound is introduced below., Formula: C9H7BrN2O2

7-bromo-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione (11.8 g, 46.2 mmol) was transferred to a round bottom flask. THF (0.57M) was added to the flask to make a slurry. Lithium aluminum hydride in 1M solution of THF (138.8 mmol) was added dropwise. When the addition was completed, the reaction mixture was heated to 63 C. After 19 hours, the reaction mixture was cooled to room temperature and then to 0 C. Water (3 mL) was added to the cooled reaction mixture, and the reaction mixture was stirred for 1 hour. After the 1 hour, 9 mL of 15% NaOH was added and the reaction mixture was stirred for another hour. Water was then added and the resulting precipitate was filtered off. The precipitate was then washed with ethyl acetate several times. The solvent was removed from the filtrate and the filtrate was transferred to a separatory funnel with ethyl acetate. The filtrate was extracted with ethyl acetate (3¡Á). The combined organic extracts were washed with brine (1¡Á), dried with magnesium sulfate, filtered and concentrated to give a yellow solid. Further purification (1% TEA/Ethyl acetate to start, then switched to 20% ammonia (2M solution in methanol)/ethyl acetate, then 100% methylene chloride) yielded the desired product. [0179] 1H NMR (CDCl3, 400 MHz): delta7.2(s,1H); 7.1 (dd, J=4, 8 Hz, 1H); 6.6(d, J=8 Hz, 1H); 3.8 (s, 2H); 3.0 (dt, J=8 Hz, 4H). [0180] Mass Spec: Calculated: 227.10; Found: 226.96 [M+H]+

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; Wyeth; US2004/9970; (2004); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics