Introduction of a new synthetic route about 2736-23-4

The synthetic route of 2,4-Dichloro-5-sulfamoylbenzoic acid has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 2736-23-4, name is 2,4-Dichloro-5-sulfamoylbenzoic acid, 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 2736-23-4

SOCl2 (2.0 ml 28 mmol) was added dropwiseto a solution of 2,4-dichloro-5-sulfamoyl-benzoic acid 3 (1.50 g5.56 mmol) in DMF (4.3 ml) at 10 C. The reaction mixture wasstirred at room temperature for 2 h and then poured on ice; theresulted precipitate was filtered off and washed with water untilpH 7 was reached. Yield 77%, mp 254-255 C. 1H NMR d ppm:2.94 (3H, s, CH3N), 3.19 (3H, s, CH3N), 7.92 (1H, s,C3-H), 8.27 (1H,s,NC-H), 8.41 (1H, s,C6-H). 13C NMR d ppm: 35.8, 41.5, 130.2,132.1, 133.9, 134.6, 136.9, 139.1, 161.3, 165.2. HRMS calcd. for C10-H10Cl2N2O4S [(M+H)+]: 324.9811, found: 324.9814.

The synthetic route of 2,4-Dichloro-5-sulfamoylbenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Article; ?apkauskait?, Edita; Zak?auskas, Audrius; Ruibys, Virginijus; Linkuvien?, Vaida; Paketuryt?, Vaida; Gedgaudas, Marius; Kairys, Visvaldas; Matulis, Daumantas; Bioorganic and Medicinal Chemistry; vol. 26; 3; (2018); p. 675 – 687;,
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The origin of a common compound about 50667-69-1

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 50667-69-1.

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. 50667-69-1, name is 2,2,2-Trifluoro-N-(hydroxymethyl)acetamide, This compound has unique chemical properties. The synthetic route is as follows., name: 2,2,2-Trifluoro-N-(hydroxymethyl)acetamide

Intermediate 1 Preparation of 2-chloro-5-((2,2,2-trifluoroacetamido)methyl)benzoic acid To a solution of 2-chlorobenzoic acid (930.0 gm,5.96 mol) in cone, sulphuric acid (5580 ml), 2,2,2-trifluoro-N-(hydroxymethyl)acetamide (930.0 gm ,6.0 mol) was added at 20 C and the reaction mixture was stirred for 15.0 h at 25-30 C. After the completion of the reaction, the reaction was slowly quenched with cold water (37.0 lit) at 10-15 C. The precipitated product was filtered and dried. The obtained product was purified using mixture of toluene and methylethylketone (7:1 x 4 times) to obtain 580.0 gm of the tittle compound having chemical purity of 98.0%, determined by HPLC.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 50667-69-1.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; MUTHUKAMAN, Nagarajan; GHARAT, Laxmikant Atmaram; KADAM, Suresh Mahadev; GAVHANE, Sachin; KHANDAGALE, Sandeep Bandu; NIRGUDE, Sunil Pandurang; (59 pag.)WO2016/199104; (2016); A1;,
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Continuously updated synthesis method about 858671-91-7

The synthetic route of 858671-91-7 has been constantly updated, and we look forward to future research findings.

Electric Literature of 858671-91-7, These common heterocyclic compound, 858671-91-7, name is tert-Butyl 2,5-Diazabicyclo[2.2.2]octane-2-carboxylate, 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.

Anhydrous dimethylacetamide (655 mL, degassed prior to use) was added to a mixture of 5 -chloro-3 -methyl- 1 -(4,4,4-trifluoro-2,2-dimethylbutyl)- 1 ,3-dihydro-2H-imidazo[4,5- ¡ê]pyridin-2-one (34-2, 175 mg, 0.544 mmol), potassium phosphate tribasic (231 mg, 1.09 mmol), bis(tri-t-butylphosphine)palladium(0) (11.2 mg, 0.02 mmol), and tert-butyl-2,5- diazabicyclo[2.2.2]octane-2-carboxylate (115 g, 0.54 mmol). The resulting suspension was heated to 100 C for 18 h. Following this duration, the reaction contents were cooled to room temperature, filtered, and washed with acetonitrile. Purification using normal-phasechromatography (40% EtOAc in hexane) afforded tert-butyl 5-[3-methyl-2-oxo-l -(4,4,4- trifluoro-2,2-dimethylbutyl)-2,3-dihydro-lH-imidazo[4,5-?]pyridin-5-yl]-2,5- diazabicyclo[2.2.2]octane-2-carboxylate (34-3) as a white solid. MS m/z (Mu+Eta): calculated = 497.5; observed = 498.5.

The synthetic route of 858671-91-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; LAYTON, Mark, E.; PERO, Joseph, E.; RODZINAK, Kevin, J.; ROSSI, Michael, A.; WO2011/34741; (2011); A1;,
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Discovery of 360773-84-8

According to the analysis of related databases, 360773-84-8, 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. 360773-84-8, name is tert-Butyl (1-(4-bromophenyl)cyclopropyl)carbamate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: tert-Butyl (1-(4-bromophenyl)cyclopropyl)carbamate

General procedure: Compound 3a (1.42g, 4.73mmol) in a 3.0N HCl solution in MeOH (10mL) was stirred at rt for 24h. The solvent was removed under reduced pressure. The resulting residue was then suspended in DCM and basified by a 2.0N solution of NaOH (20mL). The organic phases were then separated and combined and dried by anhydrous magnesium sulfate. The solvent was then removed and the residue was purified by column chromatography with pre-packed silica gel disposable column to afford the title compound 1a (1.12g, 99%) as a brown foam.

According to the analysis of related databases, 360773-84-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Dehui; Zheng, Hongchao; Wang, Xiaodong; Tetrahedron; vol. 72; 16; (2016); p. 1941 – 1953;,
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Simple exploration of 35303-76-5

According to the analysis of related databases, 35303-76-5, 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. 35303-76-5, name is 4-(2-Aminoethyl)benzenesulfonamide, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C8H12N2O2S

General procedure: To a cooled solution of triphosgene (1.41mmol) in THF at 0¡ãC, a mixture of primary amine (3.52mmol) and N,N-diisopropylethylamine (DIPEA, 7.04mmol) was added. The reaction mixture was stirred at the same temperature for 30min and then the other amine (3.52mmol) was added. The reaction mixture was slowly allowed to attain ambient temperature and further stirred for 8h. After the completion of the reaction, water was added to the reaction mixture and extracted using ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and evaporated under reduced pressure. The crude mixture was subjected to column chromatography to obtain the pure compounds.

According to the analysis of related databases, 35303-76-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Manickam, Manoj; Jalani, Hitesh B.; Pillaiyar, Thanigaimalai; Boggu, Pulla Reddy; Sharma, Niti; Venkateswararao, Eeda; Lee, You-Jung; Jeon, Eun-Seok; Son, Min-Jeong; Woo, Sun-Hee; Jung, Sang-Hun; European Journal of Medicinal Chemistry; vol. 143; (2018); p. 1869 – 1887;,
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A new synthetic route of 7341-96-0

Statistics shows that Propiolamide is playing an increasingly important role. we look forward to future research findings about 7341-96-0.

Synthetic Route of 7341-96-0, These common heterocyclic compound, 7341-96-0, name is Propiolamide, 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.

Example 2.1: Ethyl 2-{2-ethoxy-2-oxoethyl)-6-oxo-1,6-dihydropyridine-3- cartooxylate; Propiolamide (20.0 g, 289.6 mmol), diethyl 3-oxopentanedioate (87.8 g, 434.4 mmol) and sodium carbonate (24.6 g, 231.7 mmol) were mixed in water (800 mL) at 0 0C and then warmed to r.t. over 4 hours. The reaction was allowed to continue t? stir at r.t. for 3 days. The reaction was neutralized with aqueous hydrochloric acid (5M) at 0 0C with vigorous stirring. A solid precipitate was collected by filtration and washed with diethyl ether/hexanes (2:1) to yield a first batch of the title compound (43g). The filtrate was further extracted with ethyl acetate and the combined organic phases were dried over sodium sulphate and purified by column chromatography (10-80% ethyl acetate/hexanes) to yield another batch of the title compound (7g), in total gave 50 g (68%). 1H NMR (300 MHz, CDCI3): delta(ppm) 13-12 (br S, 1 H)1 8.08 (d, 1H), 6.52 (d, 1H), 4.3 (q, 2H), 4.21 (q, 2H)1 4.13 (s, 2H)1 1.29 (m, 6H).

Statistics shows that Propiolamide is playing an increasingly important role. we look forward to future research findings about 7341-96-0.

Reference:
Patent; NPS ALLELIX CORP.; WO2008/9125; (2008); A1;,
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New learning discoveries about 6973-09-7

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Amino-2-methylbenzenesulfonamide, and friends who are interested can also refer to it.

Reference of 6973-09-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 6973-09-7 name is 5-Amino-2-methylbenzenesulfonamide, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To a mixture of 5-amino-2-methylbenzenesulfonamide (20 gm) in ethanol (208 ml) and tetrahydrofuran (52 ml) was added 2,4-dichloropryrimidine (44 gm) and sodium bicarbonate (36 gm) at room temperature. The contents were heated to 70 to 75¡ã C. and maintained for 13 hours. The reaction mass was then cooled to 10¡ã C. and maintained for 2 hours. The reaction mass was filtered and the solvent was distilled off under vacuum at below 50 to 55¡ã C. to obtain a residual mass. To the residual mass was added ethyl acetate (100 ml) and stirred for 1 hour, filtered. The solid obtained was dried to give 15.5 gm of 5-(4-chloropyrimidin-2ylamino)-2-methylbenzenesulfonamide

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Amino-2-methylbenzenesulfonamide, and friends who are interested can also refer to it.

Reference:
Patent; HETERO RESEARCH FOUNDATION; Reddy, Bandi Parthasaradhi; Reddy, Kura Rathnakar; Reddy, Dasari Muralidhara; Rao, Thungathurthy Srinivasa; Krishna, Bandi Vamsi; US2013/245262; (2013); A1;,
Amide – Wikipedia,
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Some tips on 122334-37-6

The synthetic route of 122334-37-6 has been constantly updated, and we look forward to future research findings.

Electric Literature of 122334-37-6, A common heterocyclic compound, 122334-37-6, name is 4-Chloro-N-methoxy-N-methylbenzamide, molecular formula is C9H10ClNO2, 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.

Into a 250-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 6-bromo-4-(tert-butoxy)quinazoline (2.5 g, 8.89 mmol, 1.00 equiv) in tetrahydrofuran (100 mL). This was followed by the addition of n-BuLi (4.25 mL, 1.20 equiv) dropwise with stirring at -78 C. After 40 mins, to the mixture was added a solution of 4-chloro-N-methoxy-N-methylbenzamide (2.17 g, 10.87 mmol, 1.20 equiv) in tetrahydrofuran (20 mL). The resulting solution was stirred for another 30 min at 0 C. in a water/ice bath. The reaction was then quenched by the addition of water (10 mL), and concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:5), to yield of 4-(tert-butoxy)-6-[(4-chlorophenyl)carbonyl]quinazoline as a white solid.

The synthetic route of 122334-37-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; Macielag, Mark Joseph; Zhang, Yue-Mei; DeCorte, Bart L.; Greco, Michael N.; (118 pag.)US2016/68512; (2016); A1;,
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Simple exploration of 129686-16-4

The synthetic route of 129686-16-4 has been constantly updated, and we look forward to future research findings.

Electric Literature of 129686-16-4, These common heterocyclic compound, 129686-16-4, name is 6-Bromo-3,4-dihydro-1H-[1,8]naphthyridin-2-one, 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. Synthesis of the intermediates Example A.1 a) Preparation of intermediate (1) A solution of 6-bromo-3,4-dihydro-lH-[l,8]naphthyridin-2-one (1.0 g, 4.4 mmol), tert- butyl acrylate (2.56 ml, 17.62 mmol) and N,N-diisopropylethylamine (1.46 ml, 8.81 mmol) in acetonitrile (20 ml) and DMF (7 ml) was stirred and degassed with nitrogen gas for 10 minutes. Tri-o-tolylphosphine (0.27 g, 0.88 mmol) and palladium (II) acetate (47% on Pd) (0.099 g, 0.44 mol) were added and the resulting mixture was microwaved (1600 W, 180C, 35 minutes). The reaction mixture was evaporated till dryness, taken up in a mixture of DCM/methanol (8/2) (50 ml), filtered through a short pad of celite and washed with DCM. The organic layer was washed with water, dried (MgS04), filtered and evaporated to dryness. The residue was taken up in cold ethanol (10 ml) and stirred at 5C for 5 minutes, the precipitate was filtered off, washed with cold ethanol (3 ml) and dried under vacuum to yield 950 mg intermediate (1).

The synthetic route of 129686-16-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN R&D IRELAND; GUILLEMONT, Jerome, Emile, Georges; LANCOIS, David, Francis, Alain; MOTTE, Magali, Madeleine, Simone; KOUL, Anil; BALEMANS, Wendy, Mia, Albert; ARNOULT, Eric, Pierre, Alexandre; WO2013/21054; (2013); A1;,
Amide – Wikipedia,
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Extracurricular laboratory: Synthetic route of 141449-85-6

The synthetic route of 141449-85-6 has been constantly updated, and we look forward to future research findings.

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. 141449-85-6, name is tert-Butyl hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate, A new synthetic method of this compound is introduced below., SDS of cas: 141449-85-6

A 50-mL round-bottom flask was charged with 2-fluoro-4-(trifluoromethyl)benzaldehyde (0.500 g, 2.60 mmol, 1.00 equiv) in dimethyl sulfoxide (10 mL), tert-butyl octahydropyrrolo[3,4-c]pyrrole-2-carboxylate (0.828 g, 3.90 mmol, 1.50 equiv), and potassium carbonate (1.08 g, 7.81 mmol, 3.00 equiv). The resulting solution was stirred overnight at 90 C. and quenched with water (20 mL). The mixture was extracted with ethyl acetate (3*20 mL) and the organic layers were combined, washed with brine (2*20 mL), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was chromatographed on a silica gel column with ethyl acetate/petroleum ether (1/3) to provide 0.580 g (58% yield) of tert-butyl 5-(2-formyl-5-(trifluoromethyl)phenyl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate as a yellow solid. LCMS (ESI, m/z): 385 [M+H]+.

The synthetic route of 141449-85-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABIDE THERAPEUTICS, INC.; GRICE, Cheryl A.; BUZARD, Daniel J.; SHAGHAFI, Michael B.; WEBER, Olivia D.; (127 pag.)US2019/202801; (2019); A1;,
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