Amides-buliding-blocks

Related Products of 1346674-23-4, 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. 1346674-23-4, name is 7,7-Dimethyl-2,3,4,6,7,8-hexahydro-1H-cyclopenta[4,5]pyrrolo[1,2-a]pyrazin-1-one belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

0298] Example 10B (0458) [0299] Compound 170 was prepared from compounds 160 and 100 as follows: (0459) (0460) [0300] Potassium carbonate (20.3 g, 1.5 eq., 147 mmol), compound 100 (19 g, 1.1 eq., 108 mmol), compound 160 (20 g, 1 eq., 97.9 mmol), DPPF ligand (2.2 g, 0.04 eq., 3.9 mmol), and Pd(OAc)2 catalyst (0.44 g, 0.02 eq., 2 mmol) were charged to a reactor. THF (200 mL, 10 mL/g) was charged to the reactor with agitation. The reactor was evacuated and filled with N2 three times and the contents were then heated to 68C with reflux. The reactor was sampled at 22 hours and the compound 160 content was 0.9 area% by HPLC. The reactor contents were cooled to 65C and water (200 mL, 10 mL/g) was charged to the reactor over 4 hours and the reactors contents were then held at 20C for a minimum of 3 hours. The reactor contents were filtered and compound 170 was collected as a solid. The solid compound 170 was rinsed with THF/water (1 : 1 mixture, 200 mL, 10 mL/g). The washed solids were dried under vacuum with N2 purge at 22 C for a minimum of 3 hours. A yield of 84% was obtained with 99 area% by HPLC (245 nm), 79 ppm Pd and 0.2% residue on ignition (“ROI”). Of the impurities, 0.51 A% regioisomer and 0.33%> bis-coupling product were found: (0461) (0462) Regioisomer Bis-Coupling Impurity (0463) [0301] The method was repeated on a 40 g scale (based on compound 160). The coupling reaction was performed using compound 100 (1.1 eq.), Pd(OAc)2 (0.02 eq.), dppf in THF (0.04 eq., 10 mL/g) at 68 C for 28 h to reach 98.4% conversion. Water was added (350 mL) to the reaction mixture over 3 h and aged at 65 C for 10 h, cooled to 20 C in 1.5 h and aged for 16 h. After filtration and drying, a beige solid compound 170 was obtained (57.2 g, 85%, 98.6A%, 0.55A% regioisomer, 0.48A% bis-coupling impurity, 87 ppm Pd and 0.3% ROI). (0464) [0302] The method was repeated on a 609 g scale (based on compound 160). (0465) Potassium carbonate (0.6114 kg, 1.5 eq., 4.34 mol), compound 100 (0.7769 kg, 1.5 eq., 4.41 mol), compound 160 (0.6099 kg, 1 eq., 2.99 mol), DPPF ligand (0.0662 kg, 0.04 eq., 0.119 mmol), and Pd(OAc)2 catalyst (0.0137 kg, 0.02 eq., 0.061 mmol) were charged to an isolator. A reactor was evacuated and filled with N2 three times and charged with the contents of the isolator. THF (10.35 kg, 20 L/kg) was charged to the reactor with agitation. The reactor contents were heated to 68C with reflux. The reactor was sampled at 40 hours and the compound 160 content was 0.3 area% by HPLC. The reactor contents were cooled to 65C and water (6.01 kg, 10 L/kg) was charged to the reactor over 3 hours and the reactor contents were then held at 20C for a minimum of 3 hours. The reactor contents were filtered and compound 170 was collected as a solid. The solid compound 170 was rinsed with THF/water (1 : 1 mixture, 6 L, 10 mL/g). The washed solids were dried under vacuum with N2 purge at 22C for a minimum of 10 hours. A 84% yield (0.8576 kg) was obtained with 99.2 A% by HPLC (245 nm), 24 ppm Pd and less than 0.1% ROI.

The synthetic route of 7,7-Dimethyl-2,3,4,6,7,8-hexahydro-1H-cyclopenta[4,5]pyrrolo[1,2-a]pyrazin-1-one has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; BEAUDRY, Danial; CRAVILLION, Theresa; GOSSELIN, Francis; LIM, Ngiap-Kie; MALHOTRA, Sushant; TIAN, Qingping; ZHANG, Haiming; GMEHLING, Alexander; FETTES, Alec; BACHMANN, Stephan; (130 pag.)WO2018/109050; (2018); A1;,
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Application of 14719-21-2, A common heterocyclic compound, 14719-21-2, name is 2,2,2-Trifluoro-N-(prop-2-yn-1-yl)acetamide, molecular formula is C5H4F3NO, 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 solution of compound 61 (80 mg, 0.13 mmol), N-propargyltrifluoroacetylamide (196 mg, 1.30 mmol), tetrakis(triphenylphosphine)-palladium(0) (30 mg, 0.026 mmol), Cul (9.9 mg, 0.052 mmol), and Et3N (80 muGamma) in anhydrous DMF (3.0 mL) was stirred at 50C for 12 hours. The mixture was concentrated in vacuo and the residue was purified by silica gel column chromatography to yield 5-{(5)-l-[5-methoxy-4-(3-trifluoroacetamido-l-propynyl)-2-nitrophenyl]-2,2-dimethyl-propyloxy}methyl-2′-deoxyuridine 62 (75 mg, 90%). 1H NMR (400 MHz, MeOD-d4): 5 8.1 1 (s, 1 Eta, Eta-6), 8.08 (s, 1 Eta, Ph-H), 7.36 (s, 1 H, Ph-H), 6.27 (t, 1 H, J = 6.4 Hz, Eta-Gamma), 5.33 (s, 1 H, Ph-CH), 4.47 (m, 1 H, H-3′), 4.44 (s, 2 H, 5-CH2), 4.32 (d, 2 H, J = 2.0 Hz, CH2), 4.08 (s, 3 H, OCH3), 3.99 (m, 1 H, H-4′), 3.87 (m, 1 H, H-5’a), 3.79 (m, 1 H, H-5’b), 2.30 (m, 2 H, H-2), 0.93 (s, 9 H, C(CH3)3).

The synthetic route of 14719-21-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LASERGEN, INC.; STUPI, Brian, Philip; LI, Hong; WU, Weidong; HERSH, Megan, N.; HERTZOG, David; MORRIS, Sidney, E.; METZKER, Michael, L.; WO2013/40257; (2013); A1;,
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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 915087-25-1 as follows. HPLC of Formula: C8H9FN2O

Synthesis of 4-(2-cyano-2-hexadeuteropropylamino)-2-fluoro-N-methyl benzamide (compound 28) TMSCN (2.1 g, 21.2 mmol), compound 5 (0.7 g, 4.2 mmol) and deuterated acetone (1.5 g, 23.4 mmol) were placed in a microwave reaction tube, and the mixture was heated to 80C by microwave, and reacted for 3 h, power 50 W. The mixture was cooled to room temperature, deuterated acetone was removed under reduced pressure, and water was added (20 mL). The resulting mixture was extracted with ethyl acetate, washed with brine, dried over sodium sulfate, and concentrated. The resulting solid was washed with petroleum ether (10 mL) and dried by suction to give compound 28 as a white solid (870 mg, 86.6% yield). 1H NMR (CDCl3, 400 MHz): delta(ppm) 7.98 (1H, t, J = 8.4 Hz), 6.64 (1H, s), 6.62 (1H, d, J = 4 Hz), 6.58 (1H, s), 4.37 (1H, s), 3.00 (3H, s).

According to the analysis of related databases, 915087-25-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HC Pharmaceutical Co., Ltd.; CHEN, Yuanwei; EP2792674; (2014); 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. 24167-56-4, name is 4-Fluoro-N,N-dimethylbenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 4-Fluoro-N,N-dimethylbenzamide

EXAMPLE 7 A solution of 758 mg. of N,N-dimethyl-4-fluorobenzamide and 0.44 ml. of phosphorous oxychloride in 50 ml. of 1,2-dichloroethane is refluxed for one hour. To this solution is added a solution of 500 mg. of isopropyl 5,6,7,8-tetrahydropyrrolo[1,2-a]pyridine-8-carboxylate in 10 ml. 1,2-dichloroethane. The reaction mixture is refluxed for 3 hours. A solution of 3.3 g. sodium acetate trihydrate in 9 ml water is added and refluxed for a further 10 hours. The organic phase is separated, washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated to dryness. The residue is purified by preparative t.l.c. using hexane:ethyl acetate (90:10). Crystallization from dichloromethane-hexane yields isopropyl 3-p-fluorobenzoyl-5,6,7,8-tetrahydropyrrolo[1,2-a]pyridine-8-carboxylate (XI, R=H, L=p-F, R2 =iC3 H7, n=1), m.p. 92 C.

The synthetic route of 24167-56-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Syntex (U.S.A.) Inc.; US4410534; (1983); A;,
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Some common heterocyclic compound, 112257-19-9, name is tert-Butyl methyl(2-(methylamino)ethyl)carbamate, molecular formula is C9H20N2O2, 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. category: amides-buliding-blocks

N-(4-ftuoro-2-methoxy-5-nitrophenyl)-4-(1H-indol-3-yl)pyrimidin-2-amine (1.3 g, 3.43 mmol), DIPEA (2.2 gl, 7.14 mmol) and tert-butyl methyl(2-(methylamino)ethyl)carbamate (0.77 g, 4.12 mmol) were dissolved in DMA (15 mL). After heating up to 100 ¡ãC overnight, the reaction solution was concentrated and purified by column chromatography to obtain tert-butyl {2-[(4-{[4-(1H-indol-3-yl)pyrimidin-2-yl]amino}-5-methoxy-2-nitrophenyl)(methyl)am ino]ethyl}methylcarbamate (1.9 g, 80percent).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 112257-19-9, its application will become more common.

Reference:
Patent; Shanghai Hansoh Biomedical Co., Ltd.; Jiangsu Hansoh Pharmaceutical Group Co., Ltd.; WEI, Mingsong; SUN, Guangjun; TAN, Songliang; GAO, Peng; WANG, Shaobao; XIU, Wenhua; ZHANG, Fujun; BAO, Rudi; (183 pag.)EP3205650; (2017); A1;,
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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. 1280210-80-1, name is MK-3102 interMediate3, This compound has unique chemical properties. The synthetic route is as follows., name: MK-3102 interMediate3

To a solution of 11 (260 mg, 0.69 mmol) in DMAc (1 mL) was added Ml (288 mg, 0.84 mmol) followed by Ets (0.15 mL, 1.04 mmol) and stirred it for 5 minutes. AcOH (0.10 mL, 1.74 mmol) was added to the reaction mixture and continued the stirring for 30 minutes. NaBH(OAc)3 (0.44 g, 2.09 mmol) was added to the reaction mixture and continued the stirring for 2 days. The reaction mixture was quenched with NH4OH and extracted with EtOAc. Combined organics were concentrated under vacuum. Crude mixture was purified by silica gel chromatography afforded 12. XH NMR (400 MHz, CDC13): delta 7.68 (br. s., 1H), 7.36 – 7.48 (m, 1H), 7.17 – 7.30 (m, 2H), 7.05 (dt, J= 4.40, 8.80 Hz, 1H), 6.91 (d, J= 7.04 Hz, 2H), 6.69 (ddd, J= 3.08, 5.50, 8.73 Hz, 1H), 4.65 (br. s., 1H), 4.55 (br. s., 1H), 4.29 (d, J= 8.22 Hz, 1H), 4.04 (br. s., 2H), 3.59 – 3.82 (m, 2H), 3.30 (s, 3H), 2.47 (br. s., 1H), 1.93 – 2.05 (m, 1H), 1.39 (s, 9H).; Molecular Formula: C27H30F2N4O4S; LCMS purity: 84.2%; Expected: 544.2; Observed: 545.2 (M+l).

According to the analysis of related databases, 1280210-80-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK SHARP & DOHME CORP.; BIFTU, Tesfaye; WO2014/18350; (2014); 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. 406233-31-6, name is 4-Fluoro-3-nitrobenzenesulfonamide, A new synthetic method of this compound is introduced below., name: 4-Fluoro-3-nitrobenzenesulfonamide

General procedure: To an ice cold stirred solution of compound 4a-4u (1 eq) in anhydrousDCM (10 mL for 1 mmol of substrate), TEA (3 eq) was added dropwise and stirred for 10 min. Compound 5 (1 eq) was added slowly andstirred at RT for 16 h (precipitation was observed during the reactionprogress). TLC showed completion of reaction. The reaction mixturewas concentrated under reduced pressure. Water was added to thecrude material and stirred for 30 min. Obtained solid was filtered,washed with water and dried under vacuum. The solid was trituratedwith ethyl acetate, filtered and dried under high vacuum to affordcompound 6a-v.

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; Kalisha Vali; Gundla, Rambabu; Singh, Om V.; Tamboli, Yasinalli; Di Cesare Manelli, Lorenzo; Ghelardini, Carla; Al-Tamimi, Abdul-Malek S.; Carta, Fabrizio; Angeli, Andrea; Supuran, Claudiu T.; Bioorganic Chemistry; vol. 92; (2019);,
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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. 830-43-3, name is 4-(Trifluoromethyl)benzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 4-(Trifluoromethyl)benzenesulfonamide

General procedure: In 25ml RB flask to a solution of Compound 9 (200 mg) in dry DMF (5ml), EDCI (250 mg, 1.25eq) and DMAP (130 mg,1eq) were added followed by addition of Sulfonamide (1eq). RM was stirred at RT for 4hrs. Solvent from the reaction mixture was evaporated. To the residue water was added and acidified with 6N HCl, solid precipitated out. Solid was filtered and dried. Crude solid was purified by flash chromatography eluating with 4-8% MeOH/DCM as solvent system to give pure product.

The synthetic route of 830-43-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Patil, Vikas; Kale, Manoj; Raichurkar, Anandkumar; Bhaskar, Brahatheeswaran; Prahlad, Dwarakanath; Balganesh, Meenakshi; Nandan, Santosh; Shahul Hameed; Bioorganic and Medicinal Chemistry Letters; vol. 24; 9; (2014); p. 2222 – 2225;,
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Electric Literature of 6292-59-7, These common heterocyclic compound, 6292-59-7, name is 4-(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.

To 5-(2-methoxyphenoxy)-2-(2′-pyrimidinyl)-4,6-dihydroxy pyrimidine compound of formula-4 (100 g), POCI3 (500 ml) was added. Heated the reaction mixture to 90¡ãC and stirred for 30 min. The temperature of the reaction mixture was raised to 105¡ãC and was stirred for 8 hrs. The reaction mixture was cooled to 6O0C and concentrated to obtain a residue. The reaction mixture was quenched with ice water and toluene (1200 ml) was added to it. The pH was adjusted to 8-9 with 30percent sodium hydroxide solution. The organic and the aqueous layers were separated. The aqueous layer was extracted with toluene (200 ml). The organic layers were combined, washed with water and dried. The solvent was concentrated to 1200 ml and a solution of 4-tert- butyl benzene sulfonamide (6) (48 g) in toluene (600 ml), potassium carbonate (35 g) and tetra butyl ammonium bromide (10 g) was added and the reaction mixture was heated to 50¡ãC. The reaction mixture was heated to refluxed using dean stark apparatus for 10 hrs. The reaction mixture was cooled to 25¡ãC.The solid obtained was filtered and made slurry in water. The solid was filtered, washed with water and dried. Yield: 92 g

Statistics shows that 4-(tert-Butyl)benzenesulfonamide is playing an increasingly important role. we look forward to future research findings about 6292-59-7.

Reference:
Patent; MSN LABORATORIES LIMITED; WO2009/95933; (2009); A2;,
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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 164332-88-1 as follows. Quality Control of tert-Butyl (2-(2-bromoethoxy)ethyl)carbamate

Example 5-3-1 Preparation of tert-butyl (2-{2-[{5-(2-{2-[(tert- butoxycarbonyl)amino]ethoxy}ethoxy)-2-[1 -(4-ethoxy-2,6-difluorobenzyl)-1 H-indazol-3- yl]pyrimidin-4-yl}(pyridi -4-yl)amino]ethoxy}ethyl)carbamate35 mg 2-[1 -(4-ethoxy-2,6-difluorobenzyl)-1 H-indazol-3-yl]-4-(pyridin-4-ylamino)- pyrimidin-5-ol 5-1-1 (0.074 mmol, 1.0 eq.) was dissolved in 0.6 mL DMF. 31 mg potassium carbonate (0.22 mmol, 3.0 eq.) and 20 mg tert-butyl [2-(2- bromoethoxy)ethyl]carbamate 5-2-1 (0.074 mmol, 1 .0 eq.) were added. The reaction mixture was stirred at room temperature over night. 20 mg tert-butyl [2-(2- bromoethoxy)ethyl]carbamate 5-2-1 (0.074 mmol, 1 .0 eq.) was added and the reaction mixture was stirred for 2.5 h at room temperature. Butanone was added and the organic layer was washed with brine. The aqueous layer was extracted with butanone. The combined organic layers were dried with a waterresitent filter and concentrated in vacuo. The crude product was purified by flash chromatography to provide the 85% pure target compound: 20 mg, 0.03 mmol, 34%.retention time: 1 .20 minMS ES+: 662.3 [M+H]+

According to the analysis of related databases, 164332-88-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; MENGEL, Anne; LERCHEN, Hans-Georg; MUeLLER, Thomas; BAeRFACKER, Lars; HITCHCOCK, Marion; CLEVE, Arwed; BRIEM, Hans; SIEMEISTER, Gerhard; BONE, Wilhelm; FERNANDEZ-MONTALVAN, Amaury Ernesto; SCHROeDER, Jens; MOeNNING, Ursula; HOLTON, Simon; (224 pag.)WO2016/42080; (2016); A1;,
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