Tag: M.W=100-200

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. 63920-73-0, name is 2-Amino-4,6-dimethoxybenzamide, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C9H12N2O3

This product was used in next step without further purification. To a solution of 2-dimethylaminomethyl-1H-indole-5-carbaldehyde (0.88 g crude, 4.35 mmol) and 2-amino-4,6-dimethoxy-benzamide (0.85 g, 4.35 mmol) in N,N-dimethylacetamide (15 mL) were added sodium hydrogen sulfite (58.5 wt %, 0.95 g, 5.22 mmol) and p-toluenesulfonic acid (0.99 g, 5.22 mmol). The reaction mixture was stirred at 120 C. for 5 hours under nitrogen, then cooled to room temperature, and concentrated under reduced pressure. 30% aqueous sodium carbonate (50 mL) was then added. The separated solid was filtered, washed with water (50 mL), and dried under vacuum. Crude compound was purified by the Simpliflash system (0-5% methanol in CH2Cl2 and 7 N ammonia in methanol 5% in CH2Cl2 as eluent) to give the title compound as an off-white solid. Yield: 0.83 g (50%). MP 187-188 C. 1H NMR (400 MHz, DMSO-d6): delta 11.82 (s, 1H), 11.34 (s, 1H), 8.38 (s, 1H), 7.93 (d, J=8.59 Hz, 1H), 7.40 (d, J=8.59 Hz, 1H), 6.73 (s, 1H), 6.49 (s, 1H), 6.40 (s, 1H), 3.90 (s, 3H), 3.85 (s, 3H), 3.57 (s, 2H), 2.21 (s, 6H)

According to the analysis of related databases, 63920-73-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; RVX Therapeutics Inc.; McLure, Kevin G.; Young, Peter R.; US2013/281399; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 154748-63-7, name is tert-Butyl (3-hydroxycyclobutyl)carbamate, 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 154748-63-7, Formula: C9H17NO3

c) tert-butyl (3-tosyl-cyclobutyl)-carbamate18.7 g (100 mmol) tert-butyl (3-hydroxy-cyclobutyl)-carbamate and 12.1 g (120 mmol) triethylamine are placed in 500 mL chloroform. 20.5 g (105 mmol) tosyl chloride, which is dissolved in 150 mL chloroform, is added dropwise to this solution at 00C with stirring. Then the reaction mixture is allowed to come up to 200C and stirred for a further 2 h. The organic phase is washed successively with water, with dilute hydrochloric acid, with sodium hydrogen carbonate solution and again with water. The organic phase is dried on magnesium sulphate and the solvent is eliminated in vacuo. Yield: 28.3 g MS (ESI): 342 (M +H)+

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, tert-Butyl (3-hydroxycyclobutyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WO2007/115999; (2007); A1;,
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Related Products of 57561-39-4, A common heterocyclic compound, 57561-39-4, name is tert-Butyl (2-hydroxyethyl)(methyl)carbamate, molecular formula is C8H17NO3, 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 a mixture of tert-butyl 2-hydroxyethyl(methyl)carbamate (1.75 g) obtained in Reference Example 1 and ethyl acetate (20 mL) were added pyridine (0.97 mL) and 4-dimethylaminopyridine (catalytic amount), and ethyl chlorocarbonate (1.25 mL) was dropwise added. The mixture was stirred overnight at room temperature and ethyl acetate (50 mL) was added. The mixture was washed with water (50 mL), a 5% aqueous citric acid solution (50 mL) and saturated brine (50 mL), and dried over anhydrous magnesium sulfate. After concentration under reduced pressure, a 4N hydrogen chloride – ethyl acetate solution (10 mL) was added to the residue. After stirring at room temperature for 2 hrs., diethyl ether (10 mL) was added, and the precipitated solid was collected by filtration. The solid was dried under reduced pressure to give the title compound (1.66 g) as a white solid.1H-NMR(DMSO-d6) : 1.23(3H,t,J=7.1Hz), 2.54 (3H,s), 3.16-3.22(2H,m), 4.15(2H,q,J=7.1Hz), 4.32-4.37(2H,m), 9.25 (2H,br).

The synthetic route of 57561-39-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP1607088; (2005); A1;,
Amide – Wikipedia,
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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. 98-18-0, name is 3-Aminobenzenesulfonamide, A new synthetic method of this compound is introduced below., Computed Properties of C6H8N2O2S

A solution of 1-(2-methylsulfonyl-pyrimidin-4-yl)-1H-indazole (100 mg, 0.36 mmol) and p-toluenesulfonic acid (139 mg, 0.73 mmol) in i-PrOH (4 ml) was treated with 3-aminobenzene-sulfonamide (251 mg, 1.46 mmol) in a microwave synthesizer at 150° C. for 20 min. The mixture was partitioned between water and ethyl acetate, the organic layer separated, washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The crude residue was absorbed on silica gel and purified by flash chromatography (EtOAc/hexane, gradient from 30:70 to 50:50) to afford the title compound. This residue was triturated with aqueous NaOH (1 M), the solid collected by filtration, washed with water and dried under vacuum to afford 3-(4-indazol-1-ylpyrimidin-2-ylamino)-benzenesulfonamide (50 mg, 37percent yield). MS=367 [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; Roche Palo Alto LLC; US2008/146565; (2008); A1;,
Amide – Wikipedia,
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Reference of 445-28-3, 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 445-28-3 as follows.

o-fluorobenzamide (27.88,0.2mol), high purity KOH 1(22.48,0.4 mol), Methanol (12.88,0.4 mol), DMS0 (200 mL) was added to the reactor and the reaction was stirred at 20 C for 16 hours. After completion of the reaction, 800 mL of ethyl acetate was added to the system and diluted 5 times with 200 mL of saturated brine. The organic phase was separated, dried over anhydrous sodium sulfate, filtered, evaporated to dryness, and then it was loaded onto a silica gel column to separate petroleum ether: ethyl acetate = 4: 1 (volume ratio) As eluent until the product is present, the solution containing the product is collected by steaming and evaporated to dryness, followed by drying with a vacuum chestnut to give pure o-methoxybenzamide in 80% yield.

According to the analysis of related databases, 445-28-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Ferguson (Wuhan) Biotech Company Limited; Su, ji; Hua, Rui Mao; Ouyang, Kang Le; (6 pag.)CN106565522; (2017); A;,
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Related Products of 147751-16-4, These common heterocyclic compound, 147751-16-4, name is tert-Butyl methylsulfonylcarbamate, 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.

A l-L flask was charged with 2-(diethoxyphosphorylmethyl)-4-iodo-l- methoxy -benzene (5.0 g, 13 mmol), /e/V-butyl -methylsulfonylcarbamate (7.1 g, 36 mmol), cuprous iodide (2.5 g, 13 mmol), /VJV-dimethylglycine (1.4 g, 13 mmol) and potassium phosphate tribasic (11.4 g, 52.1 mmol) and the flask was purged with nitrogen. NN- Dimethylacetamide (43 mL) was then added and the flask was purged with nitrogen again, and an empty balloon was placed on top of the reaction vessel to allow room for gas generation. The reaction was stirred at 110 C for 16 hours. The resulting mixture was diluted with 10% glycine in water and acidified to pH 1 with 1N HC1, extracted with dichloromethane (3 x 50 mL), dried with anhydrous MgS04, concentrated under reduced pressure and purified by silica gel column chromatography (0% to 10% methanol in dichloromethane) to give the title compound as a white solid (922 mg, 20% yield). LCMS (ESI+) m/z 352 (M+H)+

The synthetic route of 147751-16-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GENENTECH, INC.; F. HOFFMANN-LA ROCHE AG; CUNNINGHAM, Christian; BEROZA, Paul Powell; CRAWFORD, James John; LEE, Wendy; RENE, Olivier; ZBIEG, Jason Robert; LIAO, Jiangpeng; WANG, Tao; YU, Chen; (208 pag.)WO2020/51099; (2020); A1;,
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These common heterocyclic compound, 630-22-8, name is 2,2-Dimethylpropanethioamide, 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. Safety of 2,2-Dimethylpropanethioamide

Step C: N-{3-[5-(2-chloro-4-pyrimidinyl)-2-(l, l-dimethylethyl)-l,3-thiazol-4-yl]- 2-fluorophenyl}-2,6-difluorobenzenesulfonamide To a reactor vessel was charged N-{3-[(2-chloro-4-pyrimidinyl)acetyl]-2- fluorophenyl}-2,6-difluorobenzenesulfonamide (30 g, 1 eq) followed by dichloromethane (300 mL). The reaction slurry was cooled to ~10C and N-bromosuccinimide (“NBS”) (12.09 g, 1 eq) was added in 3 approximately equal portions, stirring for 10-15 minutes between each addition. After the final addition of NBS, the reaction mixture was warmed to ~20C and stirred for 45 min . Water (5 vol) was then added to the reaction vessel and the mixture was stirred and then the layers separated. Water (5 vol) was again added to the dichloromethane layer and the mixture was stirred and the layers separated. The dichloromethane layers were concentrated to -120 mL. Ethyl acetate (7 vol) was added to the reaction mixture and concentrated to -120 mL. Dimethylacetamide (270 mL) was then added to the reaction mixture and cooled to ~10C. 2,2-Dimethylpropanethioamide (1.3 g, 0.5 eq) in 2 equal portions was added to the reactor contents with stirring for ~5 minutes between additions. The reaction was warmed to 20-25 C. After 45 min, the vessel contents were heated to 75C and held for 1.75 hours . The reaction mixture was then cooled to 5C and water (270 ml) was slowly charged keeping the temperature below 30C. Ethyl acetate (4 vol) was then charged and the mixture was stirred and layers separated. Ethyl acetate (7 vol) was again charged to the aqueous layer and the contents were stirred and separated. Ethyl acetate (7 vol) was charged again to the aqueous layer and the contents were stirred and separated. The organic layers were combined and washed with water (4 vol) 4 times and stirred overnight at 20-25C. The organic layers were then concentrated under heat and vacuum to 120 mL. The vessel contents were then heated to 50C and heptanes (120 mL) were added slowly. After addition of heptanes, the vessel contents were heated to reflux then cooled to 0C and held for ~2 hrs. The solids were filtered and rinsed with heptanes (2 x 2 vol). The solid product was then dried under vacuum at 30C to obtain N-{3-[5-(2-chloro-4-pyrimidinyl)-2-(l, l-dimethylethyl)-l,3- thiazol-4-yl]-2-fluorophenyl}-2,6-difluorobenzenesulfonamide (28.8 g, 80%).

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

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; GRESHOCK, Joel David; HOOS, Axel; WO2015/87279; (2015); A1;,
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Synthetic Route of 758-96-3, The chemical industry reduces the impact on the environment during synthesis 758-96-3, name is N,N-Dimethylpropionamide, I believe this compound will play a more active role in future production and life.

General procedure: tert-Butyl acetate (0.14 mL; 1.0 mmol) was added to a solution of LDA (1.0 mmol) in 3 mL of dry THF at -78 C under argon atmosphere with stirring. After the solution was stirred for 10 min, a solution of vinyl sulfoxide 8 (71 mg; 0.2 mmol) in THF (1 mL) was added. The reaction mixture was stirred for 15 min and then reaction was quenched by adding saturated aq. NH4Cl. The whole mixture was extracted with CHCl3. The product was purified by silica gel column chromatography to afford adduct 9 (94 mg; 99%) as colorless oil.

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

Reference:
Article; Satoh, Tsuyoshi; Awata, Yu; Kato, Yuichi; Ogata, Shingo; Ishigaki, Masashi; Sugiyama, Shimpei; Saitoh, Hideki; Tetrahedron; vol. 67; 6; (2011); p. 1102 – 1113;,
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Some common heterocyclic compound, 67074-78-6, name is 3,4-Dihydropyrido[2,3-b]pyrazin-2(1H)-one, molecular formula is C7H7N3O, 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. Recommanded Product: 67074-78-6

A mixture of 3,4-dihydropyrido[2,3-b]pyrazin-2(1H)-one (0.477 g), 4-methoxy-2-(4-(trifluoromethoxy)phenoxy)butanoic acid (0.883 g), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.690 g), 1-hydroxybenzotriazole monohydrate (0.551 g) and N,N-dimethylformamide (15 mL) was stirred at room temperature for 2 hr. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (1.09 g). 1H NMR (300 MHz, DMSO-d6) delta 1.75-2.04 (2H, m), 3.03 (3H, s), 3.23-3.46 (2H, m), 4.25 (1H, d, J = 16.6 Hz), 4.63 (1H, d, J = 16.6 Hz), 6.15 (1H, dd, J = 7.5, 4.1 Hz), 6.94-7.08 (2H, m), 7.28 (3H, dt, J = 8.3, 2.1 Hz), 7.42 (1H, dd, J = 7.9, 1.9 Hz), 8.07 (1H, dd, J = 4.7, 1.7 Hz), 10.89 (1H, brs).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 67074-78-6, its application will become more common.

Reference:
Patent; Takeda Pharmaceutical Company Limited; NAKAMURA, Shinji; MIKAMI, Satoshi; KAWASAKI, Masanori; NOMURA, Izumi; ASHIZAWA, Tomoko; TANIGUCHI, Takahiko; EP2873669; (2015); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 7223-30-5, The chemical industry reduces the impact on the environment during synthesis 7223-30-5, name is 3-Phenylpropiolamide, I believe this compound will play a more active role in future production and life.

General procedure: A degassed solution of 3-phenylpropiolamide (5.0 mmol) and N,N-dimethylethane-1,2-diamine (5.0mmol) in DMF (6.0 mL) was added through canula to a degassed solution of thevinyl iodide (1.0 mmol), Cs2CO3 (5.0 mmol) and CuI (2.0mmol) in DMF (25.0 mL) at 23 C. After stirring for the indicated time, thereaction was quenched with water and extracted with EtOAc (x3). The combined organic layers were washedwith brine, dried over Na2SO4 and filtered. The solventwas concentrated under reduced pressure, and the residue was purified byflash chromatography as indicated.

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

Reference:
Article; Garcia-Rodriguez, Jose; Mendiratta, Saurabh; White, Michael A.; Xie, Xiao-Song; De Brabander, Jef K.; Bioorganic and Medicinal Chemistry Letters; vol. 25; 20; (2015); p. 4393 – 4398;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics