Continuously updated synthesis method about C7H13NO2

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.

Electric Literature of 7150-72-3, A common heterocyclic compound, 7150-72-3, name is tert-Butyl vinylcarbamate, molecular formula is C7H13NO2, 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: A 10 mL round-bottomed flask equipped with a rubber septum and a magnetic stir bar was charged with 1 (1.0 equiv), 2 (2.5 equiv), 3 (2.0 equiv), and fac-Ir(ppy)3 (0.01 equiv). The flask was evacuated and backfilled 3 times with N2. DMSO was then added with syringe under N2. The mixture was then irradiated by white LED strips. After completion of the reaction (6 h, as judged by TLC analysis), the mixture was poured into a separatory funnel containing sat. aq NaHCO3 (20mL) and EtOAc (20 mL). After extraction with EtOAc, the organic layer was separated, dried (Na2SO4), and concentrated under reduced pressure after filtration. The crude product was purified by flash chromatography on silica gel to afford the desired product 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:
Article; An, Xiao-De; Yu, Shouyun; Synthesis; vol. 50; 17; (2018); p. 3387 – 3394;,
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New learning discoveries about 3-Bromo-N-(tert-butyl)benzenesulfonamide

Statistics shows that 3-Bromo-N-(tert-butyl)benzenesulfonamide is playing an increasingly important role. we look forward to future research findings about 308283-47-8.

Electric Literature of 308283-47-8, These common heterocyclic compound, 308283-47-8, name is 3-Bromo-N-(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.

[0190] A suspension of intermediate 34 (0.10 g, 0.29 mmol), 3-bromo-iV-2rt-butyl- benzenesulfonamide (84 mg, 0.29 mmol), Pd2(dba)3 (15 mg, 0.016 mmol), Xantphos (20 mg, 0.035 mmol) and cesium carbonate (0.18 g, 0.55 mmol) in dioxane/DMF (3/1, 4 mL) was sealed in a microwave reaction tube and irradiated with microwave at 160 “C for 15 min. After cooling to room temperature, the cap was removed and the resulting mixture filtered and the filtered solid washed with DCM. The filtrate was concentrated and the residue purified by HPLC. The fractions were combined and poured into saturated NaHCO3 solution (30 mL). The combined aqueous layers were extracted with EtOAc (2 x 30 mL) and the combined organic layers washed with brine, dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated and the residue dissolved in minimum amount of EtOAc and liexanes added until solid precipitated. After filtration, the title compound was obtained as a white solid (20 mg, 12percent) .[0191] 1H NMR (500 MHz, DMSO-d6): delta 1.12 (s, 9H), 1.30-1.40 (m, 2H), 1.50-1.56 (m, 4H), 2.16 (s, 3H), 2.88 (t, J= 5.3 Hz, 4H), 7.17 (d, J= 7.8 Hz, IH), 7.43 (t, J= 8.0 Hz, IH), 7.59-7.60 (m, 2H), 7.58 (s, IH), 8.13 (s, IH), 7.16 (dd, J= 7.9, 1.9 Hz, IH), 8.18-8.22 (m, IH), 8.67 (s, IH), 9.37 (s, IH). MS (ES+): m/z 559 (M+H)+.

Statistics shows that 3-Bromo-N-(tert-butyl)benzenesulfonamide is playing an increasingly important role. we look forward to future research findings about 308283-47-8.

Reference:
Patent; TARGEGEN, INC.; WO2007/53452; (2007); A1;,
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Extended knowledge of C12H17NO4

The synthetic route of 114790-39-5 has been constantly updated, and we look forward to future research findings.

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. 114790-39-5, name is Benzyl (2,2-dimethoxyethyl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 114790-39-5

A solution of benzyl N-(2,2-dimethoxyethyl)carbamate (50 g, 208.9 mmol) in toluene (180 mL) is treated with solid potassium hydroxide (51.6 g, 919.69 mmol) under nitrogen. After 10 minutes, benzyltriethylammonium chloride (0.8 g, 3.1 mmol) is added. After another 10 minutes a solution of allyl bromide (33 g, 272.8 mmol) in toluene (50 mL) is added drop wise over 10 minutes. The resultant mixture is stirred at 50 C for 48 hours. The mixture is cooled to room temperature and quenched with water. The organic layer is separated, washed with brine, dried over magnesium sulfate, and concentrated to dryness to give the title compound (44 g, 75%). ES/MS (m/e): 280 (M+H).

The synthetic route of 114790-39-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; COATES, David Andrew; LOSADA, Pablo Garcia; (46 pag.)WO2016/43996; (2016); A1;,
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Discovery of Dodecanamide

Statistics shows that Dodecanamide is playing an increasingly important role. we look forward to future research findings about 1120-16-7.

Synthetic Route of 1120-16-7, These common heterocyclic compound, 1120-16-7, name is Dodecanamide, 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.

Under argon atmosphere, 60.04 mmol of catalyst Nd2Na8 (OCH2CF3) 14 (THF), 1 mmol of lauric amide and 1.2 mmol of benzylamine were added into the reaction flask treated with dehydration and deoxygenation under argon atmosphere, and the mixture was stirred at 120 C. for 16 hours. The reaction was completed The reaction mixture was extracted with dichloromethane, extracted three times, and the organic phase was dried over anhydrous sodium sulfate. The solvent was drained and the residue was subjected to column chromatography (eluent: petroleum ether: ethyl acetate = 6: 1) to give The target product, N-benzyl lauramide, is a colorless solid in 90% yield.

Statistics shows that Dodecanamide is playing an increasingly important role. we look forward to future research findings about 1120-16-7.

Reference:
Patent; Anhui University; Sheng Hongting; Zeng Ruijie; Feng Yan; Zhu Manzhou; (10 pag.)CN104961777; (2017); B;,
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Application of 2-Hydroxy-N,N-dimethylacetamide

The synthetic route of 14658-93-6 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 14658-93-6, These common heterocyclic compound, 14658-93-6, name is 2-Hydroxy-N,N-dimethylacetamide, 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.

6.2a) dimethylcarbamoylmethyl 1′-{(R)-3-(4-benzyloxy-3,5-dimethyl-phenyl)-2-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carbonyloxy]propionyl}-1,4′-bipiperidinyl-4-carboxylate 30 mg (0.29 mmol) 2-hydroxy-N,N-dimethyl-acetamide were added at RT to a solution of 200 mg (0.25 mmol) 1′-{(R)-3-(4-benzyloxy-3,5-dimethyl-phenyl)-2-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carbonyloxy]-propionyl}-1,4′-bipiperidinyl-4-carboxylic acid (Example 6.1a), 90 mg (0.28 mmol) TBTU and 80 muL (3.73 mmol) triethylamine in 1.8 mL DMF and this was stirred for 20 h at RT. The reaction mixture was poured onto saturated NaHCO3 solution, the precipitate formed was suction filtered and dried. Further purification was carried out by HPLC, the fractions containing the product were combined and lyophilised. Yield: 100 mg (47% of theory) ESI-MS: (M+H)+=851 Retention time (HPLC-MS): 3.9 min (method B)

The synthetic route of 14658-93-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Mueller, Stephan Georg; Rudolf, Klaus; Lustenberger, Philipp; Stenkamp, Dirk; Santagostino, Marco; Paleari, Fabio; Doods, Henri; Arndt, Kirsten; Schaenzle, Gerhard; US2007/72847; (2007); A1;,
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Brief introduction of 563-83-7

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.

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. 563-83-7, name is Isobutyramide, A new synthetic method of this compound is introduced below., Recommanded Product: 563-83-7

A microwave vial was charged with 5-chloro-2-(5-fluoro-3-pyridyl)-4- (0220) (trifluoromethyl)pyrimidine (120mg, 0.432 mmol), 2-methylpropanamide (94mg, 1 .08mmol), JackiePhos Pd G3 (20mg, 0.017 mmol), Cs2C03 (282mg, 0.865 mmol) and anhydrous toluene (1 mL). The reaction mixture was degassed by evacuating then purging with nitrogen (x3) and then heated at 150C for 1 hour under microwave irradiation. The reaction mixture was evaporated to dryness and purified by flash chromatography on silica gel using an EtOAc/isohexane gradient as eluent to give the desired compound (127mg, 90%) as an off-white solid. (0221) 1H NMR (400 MHz, CDCb): delta 9.92 (s, 1 H), 9.48 (s, 1 H), 8.62-8.57 (m, 1 H), 8.44-8.38 (m, 1 H), 7.52 (br s, 1 H), 2.72-2.61 (m, 1 H), 1.32 (d, 6H).

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; SYNGENTA PARTICIPATIONS AG; WAILES, Jeffrey, Steven; BRIGGS, Emma; CARTER, Neil, Brian; MORRIS, Melloney; TATE, Joseph, Andrew; (56 pag.)WO2019/57721; (2019); A1;,
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Extracurricular laboratory: Synthetic route of 72505-21-6

The chemical industry reduces the impact on the environment during synthesis 4-(Trifluoromethyl)thiobenzamide. I believe this compound will play a more active role in future production and life.

Application of 72505-21-6, 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. 72505-21-6, name is 4-(Trifluoromethyl)thiobenzamide, This compound has unique chemical properties. The synthetic route is as follows.

Example 18; Intermediate: 4-Butyl-2-(4-trifluoromethyl-phenyl)-thiazol-5- carboxylic acid methyl ester; To a solution of 3-oxo-heptanoic acid methyl ester (5.0 g, 31.6 mmol) in dry dichloromethane (80 mL) add sulfurylchloride (2.82 mL). Stir the reaction mixture at room temperature for 30 minutes then add water (20 mL) and the reaction mixture extracted five times with portions of 30 mL of dichloromethane. Wash the combined organic extracts with water, saturated aqueous solution of NaHC03 and brine and then dry over MgS04. Remove the solvent under reduced pressure to give 2-chloro-3-oxo-heptanoic acid methyl ester (6.0 g), which was used in the next step without further purification. To a solution of 2-chloro-3-oxo- heptanoic acid methyl ester (6.0 g, 31.1 mmol) in ethanol (50 mL) add 4-(trifluoromethyl) thiobenzamide (6.4 g, 31.2 mmol). Heat the reaction mixture to reflux overnight. Remove the solvent under reduced pressure and purify the residue by chromatography on silica gel (eluting with a gradient of n-heptane:ethyl acetate (100:1 to 60:1)) to give 4-butyl-2-(4- trifluoromethyl-phenyl) -thiazol-5- carboxylic acid methyl ester (7.4 g) as a yellow oil. MS (ESI) m/z 344 (M+H).

The chemical industry reduces the impact on the environment during synthesis 4-(Trifluoromethyl)thiobenzamide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; AVENTIS PHARMACEUTICALS INC.; WO2005/97762; (2005); A2;,
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Research on new synthetic routes about C14H10ClNO3S

The chemical industry reduces the impact on the environment during synthesis 3-Chloro-6,11-dihydro-6-methyl-5,5,11-trioxodibenzo[c,f][1,2]thiazepine. I believe this compound will play a more active role in future production and life.

Related Products of 26638-53-9, 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. 26638-53-9, name is 3-Chloro-6,11-dihydro-6-methyl-5,5,11-trioxodibenzo[c,f][1,2]thiazepine, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of sodium metal (115 mg, 5.00 mmol) in anhydrous MeOH (5.0 mL) was added ketone 3f (308 mg, 1.00 mmol) and the mixture was heated to 100 °C for 2 h in a sealed pressure vial. The reaction was then cooled to room temperature, diluted with water (10 mL) , and extracted with CH2CI2 (3 x 10 mL) . The combined organics were washed with water (2 x 10 mL) , dried over a^SO^ , and concentrated to yield a yellow crystalline solid. This material was recrystallized from MeOH to yield ketone 3h as white prisms (158 mg, 52percent) . NMR (500 MHz , CDCI3) delta 8.33 (dd, J = 8.1, 1.6 Hz, 1H) , 8.04 (d, J = 8.7 Hz, 1H) , 7.63 (ddd, J = 8.0, 7.3, 1.7 Hz, 1H) , 7.46 (d, J = 2.6 Hz, 1H) , 7.42 – 7.34 (m, 2H) , 7.18 (dd, J = 8.7, 2.6 Hz, 1H) , 3.96 (s, 3H) , 3.33 (s, 3H) ; 13C NMR (126 MHz, CDC13) delta 189.0, 162.8, 141.2, 139.1, 134.6, 134.5, 132.4, 128.3, 126.6, 125.5, 118.9, 110.8, 56.3, 39.4; LR-MS calcd. for CisHnlTC S [M+H]+ 304.06, found 303.91

The chemical industry reduces the impact on the environment during synthesis 3-Chloro-6,11-dihydro-6-methyl-5,5,11-trioxodibenzo[c,f][1,2]thiazepine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; KRUEGEL, Andrew C.; HENKE, Adam; GASSAWAY, Madalee M.; RIVERS, Marie-laure; JAVITCH, Jonathan A.; SAMES, Dalibor; WO2015/138791; (2015); A1;,
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Sources of common compounds: 90-16-4

The synthetic route of 90-16-4 has been constantly updated, and we look forward to future research findings.

Related Products of 90-16-4,Some common heterocyclic compound, 90-16-4, name is Benzo[d][1,2,3]triazin-4(3H)-one, molecular formula is C7H5N3O, 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 the triazin-4(3H)-one (1.0 mmol), phenylboronic acid (1.5 mmol), anhydrous Cu(OAc)2 (1.0 mmol) and Et3N (2.0 mmol) in ClCH2CH2Cl (10-15 mL) was stirred at ambient temperature for 1.0-2.0 h. Progress of the reaction was monitored by TLC. The reaction mixture was filtered through celite. The filtrate was collected, concentrated in vacuo, and the residue was purified by chromatography on silica gel using hexane/ethyl acetate to afford the desired product.

The synthetic route of 90-16-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shiva Kumar; Adepu, Raju; Sandra, Sandhya; Rambabu; Rama Krishna; Malla Reddy; Misra, Parimal; Pal, Manojit; Bioorganic and Medicinal Chemistry Letters; vol. 22; 2; (2012); p. 1146 – 1150;,
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A new synthetic route of C9H17NO3

Statistics shows that tert-Butyl (3-hydroxycyclobutyl)carbamate is playing an increasingly important role. we look forward to future research findings about 154748-63-7.

Electric Literature of 154748-63-7, These common heterocyclic compound, 154748-63-7, name is tert-Butyl (3-hydroxycyclobutyl)carbamate, 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 solution of tert-butyl (3 -hydroxycyclobutyl)carbamate (see PREPARATION 4B; 1.08 g, 3.8 mmol) in DMF (20 mL) at RT was added sodium hydride (60% wt in mineral oil) (0.18 g, 7.6 mmol). The mixture was stirred at RT for 10 min and then 3-Bromo-2-fluoro- pyridine (665 mg, 3.8 mmol) was added. The reaction mixture was stirred at RT for lh and then diluted with water (20 mL) and extracted with EtOAc (2 x 30 mL). The combined organic extracts were washed with water (10 mL) and brine (10 mL), dried over Na2S04, and filtered. The filtrate was evaporated in vacuo and the residue was purified by flash columnchromatography on silica gel (5% to 30%> EtOAc in hexanes) to give tert-butyl ((lS,3S)-3-((3- bromopyridin-2-yl)oxy)cyclobutyl)carbamate (391 mg, 1.14 mmol, 30%> yield ) as white solid. ESI-MS (M+l): 343 calc. for Ci4Hi9BrN203 342.

Statistics shows that tert-Butyl (3-hydroxycyclobutyl)carbamate is playing an increasingly important role. we look forward to future research findings about 154748-63-7.

Reference:
Patent; AMGEN INC.; ALLEN, Jennifer; FROHN, Michael; HARRINGTON, Paul; PICKRELL, Alexander; RZASA, Robert; SHAM, Kelvin; HU, Essa; WO2011/143366; (2011); A1;,
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