Amides-buliding-blocks

Reference of 4141-08-6, 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. 4141-08-6 name is 2-Amino-N-methylbenzamide, 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 solution of 2-amino-N-methylbenzamide 15.00g(0.1mol) and triethylamine 12.10g(0.12mol) in 150 mL dichloromethane was added 12.40g(0.11mol) chloroacetyl chloride in 30mL dichloromethane at room temperature for 0.5 hours. Then the reaction mixture was continued stirring at room temperature for another 2-3 hours and monitored by TLC. After the reaction was over, the mixture was concentrated under reduced pressure, the residual was filtered and washed with 50ml of 10% diluted hydrochloric acid, 50ml of saturated sodium bicarbonate solution, 50ml of water and 50ml of petroleum ether successively, then dried to give 18.90g intermediate 2-(2-chloroacetamido)-N-methylbenzamide as white solid with yield of 83.4%, m.p. 155-157C.

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

Reference:
Patent; Sinochem Corporation; Shenyang Research Institute of Chemical Industry Co., Ltd.; REN, Lanhui; LIU, Changling; WANG, Lizeng; LI, Zhinian; SUN, Xufeng; LAN, Jie; WU, Qiang; CHI, Huiwei; EP2636669; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 216961-61-4, The chemical industry reduces the impact on the environment during synthesis 216961-61-4, name is tert-Butyl (10-aminodecyl)carbamate, I believe this compound will play a more active role in future production and life.

General procedure 2. Starting compound III: S-Methyl N-cyano-N’-(2-methyl4-pyridylisothiourea. Starting compound IV: 10-t-Butoxycarbonylaminodecylamine. Purification: Flash chromatography (Eluent 1% NH3(aq) and 0-10% MeOH in CH2Cl2). The compound was obtained as a yellow oil. 13C NMR (CDCl3) delta: 158.1, 157.3, 155.5, 149.4, 146.2, 116.5, 113.5, 112.0, 77.2, 41.7, 29.4, 28.9, 28.8, 28.6, 28.6, 28.6, 28.2, 26.2, 26.1, 24.0.

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 (10-aminodecyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Leo Pharmaceutical Products, Ltd. A/S; US6346520; (2002); B1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 174799-52-1, name is tert-Butyl (2-(benzylamino)ethyl)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. name: tert-Butyl (2-(benzylamino)ethyl)carbamate

Preparation 64: Synthesis of tert-butyl 2-(N-benzyl-N-methylamino)ethylcarbamate (B)To a cooled (~5 C) solution of compound A (6.2 g, 25.0 mmol) and TEA (3.0 g, 29.7 mmol, 4.13 mL) in chloroform (50 mL) was added iodomethane (4.2 g, 29.7 mmol, 1.85 mL). The pressure tube was sealed, and the mixture stirred at ambient temperature for 20 h. The mixture was then precipitated with ether (300 mL); the white solid was filtered off and washed with ether (50 mL). The filtrate was concentrated and the residual yellow oil (5.2 g) was purified by silica gel column chromatography (2-10% MeOH gradient in DCM) to give compound B (3.3 g, 12.5 mmol, 50%) as a colorless oil. TLC Rf (DCM/MeOH 9:1): 0.55. LC-MS [M+H] 264.3 (C15H24N2O2 +H, calc: 264.4).

The synthetic route of tert-Butyl (2-(benzylamino)ethyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHARMACOFORE, INC.; JENKINS, Thomas, E.; HUSFELD, Craig, O.; SEROOGY, Julie, D.; WRAY, Jonathan, W.; WO2011/133150; (2011); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2895-21-8, name is N-Isopropyl-2-chloroacetamide, 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 2895-21-8, Application In Synthesis of N-Isopropyl-2-chloroacetamide

A mixed solution of the compound 1 (120 mg), the compound 2 (123 mg), and sodium carbonate (96 mg) in acetonitrile (5 mL) was stirred for 22 hours at 50C under argon atmosphere. The reaction mixture was cooled to room temperature, diluted with ethyl acetate, washed with water and saturated brine, and dried over Chem Elut (registered trademark). The solvent was distilled off under reduced pressure, and the resultant residue was purified by silica gel column chromatography (eluent: chloroform-ammonia water (10% methanol solution) = 90:10). The resultant residue was triturated with a mixed solvent of hexane-ethyl acetate to give the compound 3 (95 mg) as a pale yellow solid. MS (APCI) 365 [M+H]+

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

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; SAKAKIBARA, Ryo; USHIROGOCHI, Hideki; SASAKI, Wataru; ONDA, Yuichi; YAMAGUCHI, Minami; AKAHOSHI, Fumihiko; (69 pag.)EP3381904; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 683-57-8, The chemical industry reduces the impact on the environment during synthesis 683-57-8, name is 2-Bromoacetamide, I believe this compound will play a more active role in future production and life.

Example 25; 2-[4-({|2-(trifluoroniethyl)phenyl]sulfonyl}amino)piperidin-l-yl]acetamide; [0234] To a suspension of N-piperidin-4-yl-2-(trifluoromethyl)benzenesulfonamide hydrochloride salt, example 3, (74 mg, 0.21 mmol) in acetone was added potassium iodide (catalytic amount) and bromoacetamide (33 mg, 0.23 mmol). The reaction mixture was heated (500C, 16 h) and monitored by LCMS. The solvent was removed in vacuo and water was added. The product was extracted with ethyl acetate and concentrated to dryness. The crude residue was purified by flash chromatography using asolvent system comprised of dichloromethane and 10% methanolic dichloromethane (0 to 80%). The isolated free base was dissolved in ethyl acetate and treated with HCl gas to afford the hydrochloride salt of 2- [4-({[2-(trifluoromethyl)phenyl]sulfonyl}amino)piperidin-l-yl]acetamide (72 mg, 85%).[0235] MS (ESI+) m/z 366;HPLC purity 100.0%, Rtau 4.6 minutes;HRMS: calculated for C4H18F3N3O3S + H+, 366.10937; found (ESI, [MH-H]+), 366.1075;

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

Reference:
Patent; WYETH; WO2008/61016; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 1280210-80-1, The chemical industry reduces the impact on the environment during synthesis 1280210-80-1, name is MK-3102 interMediate3, I believe this compound will play a more active role in future production and life.

Step A: tert-Butyl { (2R.3S,5R)-2-(2,5-difluorophenyl)-5- [2-(methylsulfonyl)-2,6- dihydropyrrolo [3 ,4-c]pyrazol-5(4H)-yl]tetrahydro-2H-pyran-3-yl } carbamateA vessel was charged with N,N-dimethylacetamide (520.6 kg), 2-(methylsulfonyl)-2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-5-ium benzenesulfonate (intermediate 2, 30.0 kg, 86.8 mol), and tert-butyl [(2R,35)-2-(2,5-difluorophenyl)-5-oxotetrahydro-2H-pyran-3 -yl]carbamate (intermediate 1, 31.2 kg, 95.3 mol). After dissolving at room temperature, the solution was cooled to 0-10 C and sodium triacetoxyborohydride (24 kg, 113 mol) was added in four equalportions every 40 mm. The reaction was then allowed to warm to room temperature and stirred an additional 5h. The solution was then cooled to 5-15 C and water (672 kg) was added over 1- 2h. The resulting slurry was filtered and the cake washed sequentially with N,Ndimethylacetamide, twice with water, and then n-heptane. The solids were dried under vacuum at 40-60 C to give tert-butyl { (2R,3S,5R)-2-(2,5-difluorophenyl)-5 – [2-(methylsulfonyl)-2,6-dihydropyrrolo [3 ,4-cjpyrazol-5(41])-yljtetrahydro-2H-pyran-3-yl } carbamate.

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, MK-3102 interMediate3, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ARROYO, Itzia; KRUEGER, Davida; CHEN, Ping; MOMENT, Aaron; BIFTU, Tesfaye; SHEEN, Faye; ZHANG, Yanfeng; MERCK SHARPE & DOHME LTD.; WO2013/3249; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 79722-21-7, A common heterocyclic compound, 79722-21-7, name is tert-Butyl benzyloxycarbamate, molecular formula is C12H17NO3, 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.

Sodium hydride 60% dispersion in mineral oil (0.55 g, 13.7 mmol) was added portion- wise to a stirring solution of fe/f-Butyl /V-(benzyloxy)carbamate (2.05 g, 9.18 mmol) in DMF (15 mL) under a nitrogen atmosphere at ambient temperature. The reaction mixture was stirred for 15 min. 1 (3.00 g, 10.1 mmol) in DMF (10 mL) was added dropwise and the reaction mixture was stirred under a nitrogen atmosphere at ambient temperature overnight. The reaction mixture was quenched with water (100 mL) and extracted with ethyl acetate (3 x 100 mL). The organic layers were pooled, washed with brine (100 mL), dried over Na2S04 and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with 1 :4 ethyl acetate/hexane to give a yellow oil (Yield: 1 .94 g, 37%). (0296) 1 H NMR (400 MHz, CDCI3): : delta 7.78 – 7.82 (m, 2H), 7.65 – 7.70 (m, 2H), 7.29 – 7.37 (m, 5H), 4.77 (s, 2H), 3.87 (t, J = 7.2 Hz, 2H), 3.69 (t, J = 7.2 Hz, 2H), 3.60 – 3.62 (m, 2H), 3.54 – 3.57 (m, 2H), 1.45 (s, 9H); 13C NMR (101 MHz, CDCI3): delta 168.3, 156.8, 135.8, 134.1 , 132.3, 129.6, 128.6, 128.5, 123.4, 81 .5, 77.1 , 67.7, 67.3, 49.8, 37.5, 28.4.

The synthetic route of 79722-21-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE UNIVERSITY OF SYDNEY; CODD, Rachel; KATSIFIS, Andrew; LIFA, Tulip; TIEU, William; RICHARDSON-SANCHEZ, Tomas; (90 pag.)WO2017/96430; (2017); A1;,
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. 6973-09-7, name is 5-Amino-2-methylbenzenesulfonamide, A new synthetic method of this compound is introduced below., Safety of 5-Amino-2-methylbenzenesulfonamide

Example 4b: Synthesis of Pazopanib Hydrochloride (0040) To a suspension of N-(2-chloropyrimidin-4-yl)-N-2,3-trimethyl-2H-indazol-6-amine (90 g, 0.312 mol) and 5-amino-2-methyl benzene sulfonamide (64.07 g, 0.344 mol) in isopropyl alcohol (900 mL) was added 4M hydrochloric acid solution in isopropyl alcohol (1.56 mL, 6.25 mol). The reaction mixture was heated to reflux temperature for 10 hours to 12 hours. The reaction mixture was cooled to 25 C. The reaction mixture was further stirred at 25 C. to 30 C. for 30 minutes, then the solid was filtered. The wet solid was washed with isopropyl alcohol (180 mL×2), and then dried under vacuum at 45 C. to 50 C. for 12 hours to afford the hydrochloride salt of 5-({4-[(2,3-dimethyl-21-I-indazol-6-yl)(methyl) amino] pyrimidin-2-yl} amino-Z-methylbenzene sulfonamide as a light brown solid. Yield: 97% w/w.

The synthetic route of 6973-09-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sun Pharmaceutical Industries Limited; KUMAR, Rajesh; GIRI, Prabhat; BARMAN, Dhiren C.; NATH, Asok; PRASAD, Mohan; (5 pag.)US2015/329526; (2015); A1;,
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. 19047-31-5, name is 2-Chloro-N-cyclopropylacetamide, A new synthetic method of this compound is introduced below., Product Details of 19047-31-5

Compound m (148 mg) was dissolved in 5.0 ml DMF and Cs2CO3 (330 mg) was added, followed by the addition of N1-cyclopropyl-2-chloroacetamide (130 mg). The vial was capped and the reaction was heated to 70 C. in a heat block for 4 hrs. The reaction was completed by LCMS. Diluted reaction with H2O, extracted with EtOAc, dried over MgSO4, concentrated by vacuum, and flashed by ISCO (EtOAc/hexanes) to give compound o. Compound o was dissolved in 10 ml THF and cooled to 0 C. before adding 0.14 ml 2.5 M LAH in THF. The reaction was stirred 1 hr 35 min at 0 C. and was completed by LCMS. The reaction was quenched with 400 uL 10% NaOH and 400 uL EtOH, diluted with H2O and 1 M HCl, extracted with DCM, dried over MgSO4 and concentrated under vacuum to give compound p. Compound p was dissolved in 2 ml 1.0 M TBAF in THF and 3 ml THF and heated to 60 C. overnight. Reaction was completed by LCMS and diluted with H2O, extracted with EtOAc, washed with brine, dried over MgSO4, concentrated under vacuum and purified by HPLC to give 18 mg of the final compound 85.

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; Rawson, Thomas E.; Safina, Brian; Dotson, Jennafer; Zhou, Aihe; Aliagas-Martin, Ignacio; Halladay, Jason; Liang, Jun; Rueth, Matthias; Zhu, Bing-Yan; US2007/37791; (2007); A1;,
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. 19982-07-1, name is N-(3,5-Dimethyladamantan-1-yl)acetamide, A new synthetic method of this compound is introduced below., Product Details of 19982-07-1

Example 5: Memantine hydrochloride synthesis; 486g (600 ml) of n-butanol, 150 g of l-acetamido-3,5-dimethyladamantane and241 g of 89.9% potassium hydroxide are added to a 2-liter reactor equipped with a condenser, a mechanical stirrer, and a thermometer at 20-250C under nitrogen. After addition, the internal temperature rises to 40-450C without external cooling. The resulting suspension is heated to 128-132C over 20-30min and a solution is obtained. After lOhrs at 128-132C (no reflux), the reaction is complete (unreacted l-acetamido-3,5- dimethyladamantane less than 1%).After cooling to 45-500C, water (450ml) is added to form a biphasic system. After stirring (5min) and standing (15min) at 20-250C, the phases are separated. The aqueous phase is discarded and water (225ml) is added to organic phase to form a biphasic system and pH is brought to 10.5-11 with 37% hydrochloric acid (1Og). After stirring (5min) and standing (15min) at 20-250C, the phases are separated. Water (225ml) is added to the organic phase to form a biphasic system and after stirring (5min) and standing (15min) at 20-250C, the phases are separated. To the organic phase, 37% hydrochloric acid (66,9g) is added and the solution is filtered on paper filter. The obtained solution is concentrated under vacuum until a residual volume of 360 ml is obtained (a semisolid but well stirrable mixture) and internal temperature is 5O-55C. At this point, after cooling to 45-500C, ethyl acetate (750ml) is added. The obtained suspension is cooled to 0+/-3C and after 3hrs it is filtered and solid washed three times with ethyl acetate (90ml each). Wet white solid is dried under vacuum at 55-600C for 15 hrs. Dry weight: 138.7g, Yield: 95%, Purity: 99.97% by GC.

The synthetic route of 19982-07-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TEVA PHARMACEUTICAL FINE CHEMICALS S.R.L.; TEVA PHARMACEUTICALS USA, INC.; WO2007/126886; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics