Amides-buliding-blocks

Related Products of 2623-33-8, 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. 2623-33-8, name is 4-Acetamidophenyl acetate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 6 Preparation of 4-Acetoxy-2-nitroacetanilide (V) A 500 mL, Erlenmeyer flask equipped with a magnetic stirring bar and a thermocouple was charged with 4-acetoxyacetanilide (10.3 g, 0.05 mol), methylene chloride (50 mL), and acetic anhydride (16.2 g, 0.16 mol). The mixture was stirred at ambient temperature for 15 minutes (incomplete solution), and then was cooled to 0C (ice-salt bath). Nitric acid (5.0 mL, 0.08 mol, 70% acid, d=1.42) was added over a 30 second period. The ice bath was removed and the mixture was heated to boiling (42.5C) and maintained at that temperature for 30 minutes. The reaction temperature was slowly increased to 75C to distill methylene chloride, and then the mixture was allowed to cool slowly to ambient temperature and stand for 16 hours. The crystalline precipitate was isolated by filtration and vacuum dried to yield 7.1 g, 0.03 mol of 4-acetoxy-2-nitroacetanilide (mp 143-146C).

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

Reference:
Patent; IOLAB CORPORATION; EP282294; (1988); A2;,
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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. 50487-72-4, name is N,N-Diallyl-4-methylbenzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of N,N-Diallyl-4-methylbenzenesulfonamide

General procedure: A solution of 18 (0.001-0.0025 mmol, 1.00 mol%-10.0 mol%) was added to a solution of alkene (0.10 mmol) in toluene (0.10 mL; 1.0 M) under nitrogen. The resulting mixture was stirred at 100 C for 2-12 h. Then, the solvent was removed under reduced pressure to yield a crude product, which was purified by flash chromatography (c-hexane-CH2Cl2) to remove the Ru residue. Conversions were obtained as confirmed by 1H NMR spectroscopy by comparing the ratios of the integrals of the starting materials with those of the products. The catalytic activities of ruthenium carbyne 18 to a variety of substrates are shown in Table 1.

The synthetic route of 50487-72-4 has been constantly updated, and we look forward to future research findings.

Reference:
Amide – Wikipedia,
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Some common heterocyclic compound, 108-13-4, name is Malonamide, molecular formula is C3H6N2O2, 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: Malonamide

(1) Production of 1,2-dihydro-2-oxo-6-(trifluoromethyl)pyridine-3-carboxamide; Sodium methoxide (74g, 1.37 mol) was dissolved in methanol (1,000 mL), and malon diamide (100g, 0.979 mol) was added to this solution at room temperature. To this mixture, 4-ethoxy-1,1,1-trifluoro-3-buten-2-one (191g, 1.14 mol) was added dropwise at a temperature between 25 and 30C, and the resultant mixture was refluxed under heating for 2 hours. After cooling to 45C, concentrated hydrochloric acid was added to the mixed solution to give a pH of 3 to 4, and 500 mL of methanol was distilled off at normal pressure. To the residue, water (500 mL) was added, and the mixture was stirred for a day at room temperature. The resultant product was precipitated while cooling with ice. Thus obtained crystal was collected by filtration, washed with water, and then dried under reduced pressure, to obtain 167g of a subject compound (yield: 83%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 108-13-4, its application will become more common.

Reference:
Patent; KUMIAI CHEMICAL INDUSTRY CO., LTD.; IHARA CHEMICAL INDUSTRY CO., LTD.; EP1982978; (2008); A1;,
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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. 459817-82-4, name is tert-Butyl 1,2,3-oxathiazolidine-3-carboxylate 2,2-dioxide, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H13NO5S

Methyl 4-chloro-lH-pyrrolo[2,3-b]pyridine-2-carboxylate (2 g, 9.50 mmol) was taken up in DMF (30 ml), cooled to 0 C and KOtBu (1.1 g, 9.80 mmol) was added. After 30 min tert-butyl 2,2-dioxooxathiazobdine-3-carboxylate (2.3 g, 10.3 mmol) was added, the cooling bath removed, and the mixture stirred at rt for 1.5 h. Aq. 10% citric acid (50 ml) and EtOAc (30 ml) were added and the organic layer separated. The aqueous layer was extracted with EtOAc (3 x 15 ml) and the combined organics were washed with water (3 x 20 ml), brine (20 ml), dried over Na^SOr. filtered and concentrated to give the product as a gum, which solidified upon standing (2.9 g, 86%). MS ES+ m/z 354 [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; PETRA PHARMA CORPORATION; KESICKI, Edward A.; RAVI, Kannan Karukurichi; LINDSTROeM, Johan; PERSSON, Lars Boukharta; LIVENDAHL, Madeleine; VIKLUND, Jenny; GINMAN, Tobias; FORSBLOM, Rickard; RAHM, Fredrik; HICKEY, Eugene R.; DAHLGREN, Markus K.; GERASYUTO, Aleksey I.; (478 pag.)WO2019/126733; (2019); A1;,
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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. 227940-71-8, name is tert-Butyl 7-benzyl-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of tert-Butyl 7-benzyl-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate

To a solution of 3 (350 mg, 1.11 mmol) in 30mL of dry ethanol was added 28 % of the Pd, 10 wt. % on activated carbon, and H2 was bubbled through the reaction mixture for 4 hrs. The reaction was monitored by TLC. The solution was filtered through a sintered funnel and evaporated to yield 230 mg of the product 4. Yield: 92 %. (HRMS): calcd for C12H23N2O2 m/z 227.1760, found m/z 227.1750

The synthetic route of 227940-71-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Haridas; Sadanandan, Sandhya; Sharma, Yogesh K.; Chinthalapalli, Srinivas; Shandilya, Ashutosh; Tetrahedron Letters; vol. 53; 6; (2012); p. 623 – 626;,
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Some common heterocyclic compound, 478832-21-2, name is tert-Butyl 4-hydroxyazepane-1-carboxylate, molecular formula is C11H21NO3, 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. Application In Synthesis of tert-Butyl 4-hydroxyazepane-1-carboxylate

To a solution of tert-butyl 4-hydroxyazepane-i-carboxylate (3.0 g, 14.0 mmol, 1.0 equiv.) and N,N-diisopropylethylamine (3.2 mL, 18.0 mmol, 1.3 equiv.) in (1574) dichloromethane (70 mL) was added methanesulfonyl chloride (1.2 mL, 15.0 mmol, 1.1 equiv.). The reaction mixture was stirred at room temperature for 1 hour and then water was added. The organic layer was separated and then washed twice with water, once with brine, dried over sodium sulfate, filtered and concentrated in vacuo to give the title compound (3.87 g, 95 %). (1575) NMR (CDC13) delta 4-97 – 4-76 (m, 1 H), 3.62 – 3.24 (m, 4 H), 3.00 (s, 3 H), 2.14 – 1.83 (m, 4 H), 1.68 (q, 2 H), 1.45 (s, 9 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 478832-21-2, its application will become more common.

Reference:
Patent; INFLAZOME LIMITED; COOPER, Matthew; MILLER, David; MACLEOD, Angus; VAN WILTENBURG, Jimmy; THOM, Stephen; ST-GALLAY, Stephen; SHANNON, Jonathan; (352 pag.)WO2019/8025; (2019); A1;,
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22117-85-7, name is 2-Methoxy-5-sulfamoylbenzoic acid, 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. category: amides-buliding-blocks

EXAMPLE 53 N-(1-Cyclohexyl-3-pyrrolidinyl)-2-methoxy-5-sulfamoylbenzamide To 3.7 g. (0.022 mole) of 3-amino-1-cyclohexylpyrrolidine in 100 ml. of pyridine was added dropwise with cooling 1.1 g. (0.008 mole) of phosphorous trichloride at 20C. After stirring one hour, 3 g. (0.013 mole) of 2-methoxy-5-sulfamoylbenzoic acid was added and refluxed 6 hrs. The solution was concentrated and the residue partitioned between dilute hydrochloride acid and isopropyl ether. The acid was made basic with ammonium hydroxide and extracted with chloroform which was dried (sodium sulfate) and concentrated. The residue was crystallized from ethyl acetate and recrystallized from isopropyl alcohol. Yield 1 g. (33%); m.p. 184-187C. Anaylsis: Calculated for C18 H27 N3 O4 S: C,56.67; H,7.13; N,11.02. Found: C,56.39; H,7.09; N,11.00.

The synthetic route of 22117-85-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; A. H. Robins Company, Incorporated; US3966957; (1976); A;,
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Reference of 112101-81-2,Some common heterocyclic compound, 112101-81-2, name is R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide, molecular formula is C10H16N2O3S, 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 1: Preparation of 5-[(2R)-2-[[2-(2-ethoxyphenoxy)ethyl]amino]propyl]-2- methoxybenzene-sulfonamide (Tamsulosin base)(R)-5-(2-arriinopropyl)-2-methoxybenzenesurfonarnide (60 g; 245.59 mmol) and l-(2- bromoethoxy)-2-ethoxybenzene (57.25 g; 233 mmol) were dissolved in 240 mL of N5N- dimethylformamide and 50.5 mL of diisopropylethylamine. The reaction mixture was heated to 100 C and stirred for 90 minutes. The mixture was then cooled to 20 C and 720 mL of ethyl acetate and 300 mL of water added to the vessel. The mixture was then stirred for 20 minutes at atmospheric condition, and then was allowed to settle. The aqueous layer was separated and re-extracted twice with 300 mL of ethyl acetate. The organic layers were combined and washed with 600 mL of water.The organic phase (1120 mL of ethyl acetate) was then concentrated by distillation at atmospheric pressure during which a white solid was precipitated. The mixture was then cooled to 2 C and stirred for 1 hour. The resulting crystals were isolated by filtration and washed with ethyl acetate to yield 133.59 g of wet tamsulosin base (Loss on Drying: 55.08% (corresponding to 60.01 g of dry material); HPLC Purity: 95.025%).EXAMPLE 3: Preparation of 5-[(2R)-2-[[2-(2-ethoxyphenoxy)ethyl]amino]propyl]-2- methoxybenzene-sulfonamide (Tamsulosin base)(R)-5-(2-aminopropyl)-2-methoxybenzenesulfonamide (100 g; 409.31 mmol) and 1- (2-bromoethoxy)-2-ethoxybenzene (95.4 g; 388 mmol) were dissolved in 400 mL of N,N- dimethylformamide and 84 mL of diisopropylethylamine. The reaction mixture was heated to 100 C and stirred for 90 minutes. The mixture was then cooled to 20 C, and 1200 mL of ethyl acetate and 500 mL of water were added. The mixture was then stirred for 20 minutes at atmospheric conditions and was allowed to settle. The aqueous layer was then separated and re-extracted twice with 500 mL of ethyl acetate. Next, the organic layers were combined and washed with 1000 mL of water.The organic phase (~1570 mL of ethyl acetate) was then concentrated by distillation at atmospheric pressure during which a white solid was precipitated. The mixture was then cooled to 2 C, and stirred for 1 hour. The resulting crystals were isolated by filtration and washed with ethyl acetate to yield 125.93 g of wet tamsulosin base (Loss on Drying: 24.09% (corresponding to 95.59 g of dry material); HPLC Purity: 97.62%). EXAMPLE 4: Preparation of 5-[(2R)~2-[[2-(2-ethoxyphenoxy)ethyl]amino]propyI]-2- methoxybenzene-sulfonamide (Tamsulosin base)(R)-5-(2-arninopropyl)-2-methoxybenzenesulfonamide (3 g; 12.27 mmol) and l-(2- bromoethoxy)-2-ethoxybenzene (2.86 g ; 11.63 mmol) were dissolved in 12 mL of N5N- dimethylformamide and 2.55 mL of diisopropylemylamine. The reaction mixture was heated to 100 C and stirred for 90 minutes. The mixture was then cooled to 20 C, and 36 mL of ethyl acetate and 15 mL of water were added. The mixture was then stirred for 20 minutes at atmospheric conditions and was allowed to settle. The aqueous layer was then separated and re-extracted twice with 15 mL of ethyl acetate. Next, the organic layers were combined and washed with 75 mL of water.The organic phase (~80 mL of ethyl acetate) was concentrated by distillation at atmospheric pressure during which a white solid was precipitated. The mixture was then cooled to 2 C and stirred for 1 hour. The resulting crystals were isolated by filtration and washed with ethyl acetate to yield 5.14 g of wet tamsulosin base (Loss on Drying: 39.68% (corresponding to 3.1 g of dry material); HPLC Purity: 96.65%).The solid obtained in the previous step was then combined with 31 mL of ethanol. The reaction mixture was then heated to 78 C and stirred for 40 minutes, cooled to 0 C and stirred for 150 minutes. The resulting crystals were isolated by filtration to yield 4.92 g of wet tamsulosin base (Loss on Drying: 40.59% (corresponding to 2.81 g of dry material); HPLC Purity: 98.70%).

The synthetic route of 112101-81-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MEDICHEM, S.A.; WO2007/119110; (2007); A2;,
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Some common heterocyclic compound, 17641-08-6, name is 2-Chloro-N-(3-methoxyphenyl)acetamide, molecular formula is C9H10ClNO2, 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-Chloro-N-(3-methoxyphenyl)acetamide

General procedure: A mixture of the potassium salt 22 (1.5g, 0.01mol) and the appropriate chloroacetanilides (0.01mol) namely, 2-chloro-N-(3-methoxyphenyl)acetamide and 2-chloro-N- (4-fluorophenyl)acetamide in dry DMF (20ml) was heated over a water bath for 3h. The reaction mixture was then cooled, poured into ice-cooled water (150ml) and stirred well for 30min. The solid such separated was filtered, washed with water, dried and crystallized from methanol/toluene mixture (1:1) to afford the corresponding compounds 25a – b, respectively. 2-(Bis[1,2,4]triazolo[4,3-a:3?,4?-c]quinoxalin-3-ylsulfanyl)-N-(3-methoxyphenyl) acetamide (25a). White crystal (yield 71 %); m. p. 256 – 259 C; IR (KBr, cm1); 3264 (NH), 3077 (CH aromatic), 2950 (CH aliphatic), 1689 (C=O amide); 1H NMR (DMSO-d6) delta ppm: 3.70 (s, 3H, -OCH3), 4.52 (s, 2H, CH2), 6.62 (d, 1H, J=8.1Hz, Ar-H, H-4 of phenyl), 6.69 (d, 1H, J=8.4Hz, Ar-H, H-6 of phenyl), 7.20 (dd, 1H, J=8.1, 8.4Hz, Ar-H, H-5 of phenyl), 7.23 (s, 1H, Ar-H, H-2 of phenyl), 7.72 (dd, 1H, J=7.8, 8.4Hz, Ar-H, H-7 of quinoxaline), 7.74 (dd, 1H, J=7.8, 8.1Hz, Ar-H, H-6 of quinoxaline), 8.45 (d, 1H, J=8.4Hz, Ar-H, H-8 of quinoxaline), 8.59 (d, 1H, J=8.1Hz, Ar-H, H-5 of quinoxaline), 10.02 (s, 1H, Ar-H, N-CH=N), 10.54 (s, 1H, -NH, D2O exchangeable); 13C NMR (DMSO-d6, 100 MHz) delta (ppm): 38.9, 55.4, 105.4, 109.4, 111.8, 118.0, 118.5, 123.1, 124.0, 128.3 (2), 130.0, 138.7, 139.4, 140.3, 142.3, 147.7, 159.9, 165.5; DEPT (DMSO-d6, 100 MHz) delta (ppm): 38.9 (1CH3), 55.4 (1CH2), 105.3, 109.4, 111.8, 118.0, 118.5, 128.3 (2), 130.0, 138.7 (9CH); Anal. Calcd. for C19H15N7O2S (405.43): C, 56.29; H, 3.73; N, 24.18. Found: C, 56.42; H, 3.71; N, 24.39 %.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 17641-08-6, its application will become more common.

Reference:
Article; Ibrahim; Taghour; Metwaly; Belal; Mehany; Elhendawy; Radwan; Yassin; El-Deeb; Hafez; ElSohly; Eissa; European Journal of Medicinal Chemistry; vol. 155; (2018); p. 117 – 134;,
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Application of 174799-52-1, A common heterocyclic compound, 174799-52-1, name is tert-Butyl (2-(benzylamino)ethyl)carbamate, molecular formula is C14H22N2O2, 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.

41 c (5.00g, 17.96 mmol) and 56 (4.497g, 17.96 mmol, 1 eq) were dissolved in EtOH (30 mL) and a few drops of water added, before splitting the mixture into 2 x 30 mL W vessels. Each mixture was heated at 100 C for 30 mins in the MW reactor (dynamic program with maximum pressure 250 psi, maximum power 300W). Concentration of the reaction mixture gave approximately 10 g of crude residue. This was purified by FCC (eluent PE/DCM 1 :1 to prime/load the column, with the gradient increasing to 100% DCM over 5CV, 1 00% DCM for a further 3 CV and then raise to DCM/MeOH 99:1 over 1 CV, then to 95:5 over 3 CV, holding at this concentration to elute the desired product). This gave 7.30 (77%) g of white crystalline solid.

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; THE UNIVERSITY OF NOTTINGHAM; MISTRY, Shailesh; DARAS, Etienne; FROMONT, Christophe; JADHAV, Gopal; FISCHER, Peter Martin; KELLAM, Barrie; HILL, Stephen John; BAKER, Jillian Glenda; WO2012/4549; (2012); A1;,
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