Month: February 2021

Application of 167216-30-0, The chemical industry reduces the impact on the environment during synthesis 167216-30-0, name is tert-Butyl (3-hydroxybutyl)carbamate, I believe this compound will play a more active role in future production and life.

Step 2: Synthesis of tert-butyl 6-methyl-1,2,3-oxathiazinane-3-carboxylate 2-oxideTo a stirred solution of thionyl chloride (2.0 mL, 27.9 mmol) in acetonitrile (15 mL) cooled to -45 C is added a solution of tert-butyl (3-hydroxybutyl)carbamate (2.1 g, 11.2 mmol) in acetonitrile (20 mL) by syringe over 10 min, keeping the internal temperature below -40 C. 4-Dimethylaminopyridine (136 mg, 1.1 mmol) is added followed by the dropwise addition of pyridine (4.5 mL, 55.8 mmol, keeping the temperature below -40 C. The addition takes 90 min. Ethyl acetate (50mL) is added to the suspension and the mixture is filtered at -35 C to remove the solid and the solid which is washed with EtOAc before it is discarded. The filtrates are combined, and saturated Na2HP04 solution (20 mL) is added. The mixture is stirred vigorously for 30 min and the organic layer is separated, washed with 1M NaHS04 to remove residual pyridine, dried (MgS04) and concentrated to afford the title compound (2.52 g, 96%) as an oil.

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 (3-hydroxybutyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOYER, Stephen, James; GAO, Donghong, Amy; GUO, Xin; KIRRANE, Thomas, Martin, Jr.; SARKO, Christopher, Ronald; SNOW, Roger, John; SOLEYMANZADEH, Fariba; ZHANG, Yunlong; WO2011/71716; (2011); 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. 894852-01-8, name is 7-Bromo-2,2-dimethyl-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one, A new synthetic method of this compound is introduced below., name: 7-Bromo-2,2-dimethyl-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one

b) (E)-3 -(2,2-Dimethyl-3 -oxo-3 ,4-dihydro-2H-pyrido[3,2-&] [ 1 ,4]oxazin-7-yl)-iV-methyl-N- (3-methylbenzofuran-2-yhnethyl)acrylamide; A solution of N-methyl-N-(3-methylbenzofuran-2-yhnethyl)acrylamide (0.231 g,1.01 mmol) in propionitrile (4 mL) and DMF (0.8 mL) was deoxygenated with Ar for 20 min. The solution was treated with diisopropylethylamine (0.28 mL, 1.64 mmol) and 7- bromo-2,2-dimethyl-4H-rhoyrido[3,2-][l,4]oxazin-3-one (0.200 g, 0.775 mmol). The solution was deoxygenated with Ar for 20 min. Pd(OAc)2 (0.017 g, 0.078 mmol) and P(o- tol)3 (0.047 g, 0.15 mmol) were then added and the solution was deoxygenated again with Ar for 10 min. The mixture was heated to reflux for 18 h, then allowed to cool. The mixture was diluted with H2O (100 mL). The resulting solids were collected by filtration and washed with Et2O (50 mL). Residual palladium was removed by silica gel plug (silica gel, 95:5, CH2Cl2/Me0H) the resulting solution concentrated to reveal a light orange solid. The solid was triturated with Et2O and dried to give the title compound (0.14 g, 46%) as a light pink solid and as a mixture of amide rotamers: 1H NMR (300 MHz, DMSO-JPatent; AFFINIUM PHARMACEUTICALS, INC.; WO2007/53131; (2007); A2;,
Amide – Wikipedia,
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Reference of 198989-07-0, The chemical industry reduces the impact on the environment during synthesis 198989-07-0, name is tert-Butyl 2,5-diazabicyclo[2.2.1]heptane-2-carboxylate, I believe this compound will play a more active role in future production and life.

a) iert-Butyl 5-(3-bromoimidazo[1 ,2-b]pyridazin-6-yI)-2,5diazabicyclo[2.2.1]heptane-2- carboxylate3-Bromo-6-chloroimidazo[1 ,2-b]pyridazine (586 mg, 2.53 mmol) was dissolved in NMP (5 mL) and 2,5-diazabicyclo[2.2.1]heptane-2-carboxylic acid 1 ,1-dimethylethyl ester (1.0 g, 5.05 mmol) was added followed by DIPEA (1.04 mL, 6.31 mmol). The reaction mixture was heated to 30C for 4 h. The solution was cooled down and diluted with DCM, then washed twice with water and twice with brine. The solution was dried over magnesium sulphate and solvents evaporated. Purification by column chromatography on silica gel (10- 00% EtOAc/petroleum ether) gave a brown oil. This was dissolved in ethyl acetate, washed four more times with brine, dried over magnesium sulphate and the solvents evaporated to give a brown solid (486 mg, 49%); H NMR (400 MHz, CDCI3) delta ppm 7.67 (d, J=9.6 Hz, 1 H), 7.67 (d, J=9.6 Hz, 1 H), 7.52 (s, 1 H), 6.54 (d, J=9.6 Hz, 1 H), 4.49-4.84 (m, 2H), 3.43-3.67 (m, 4H), 1.94-2.07 (m, 2H), 1.48 (s, 9H); m/z (ES+APCIf: 394/396 [M+H]+.

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 2,5-diazabicyclo[2.2.1]heptane-2-carboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MEDICAL RESEARCH COUNCIL TECHNOLOGY; OSBORNE, Simon; CHAPMAN, Timothy; WALLACE, Claire; WO2012/127212; (2012); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 2227-79-4,Some common heterocyclic compound, 2227-79-4, name is Benzothioamide, molecular formula is C7H7NS, 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 ethyl bromopyruvate (0.68g, 3.5 mmol) and thiobenzamide(0.40 g, 2.9 mmol) in ethanol (25 mL) was heated to reflux for 4 h. The solvent was removed under reduced pressure, and the residue was washed with water (30ml) and extracted with ethyl acetate (3 ¡Á 20 mL). The organic layer was driedover anhydrous Na2SO4 and concentrated. The residue waspurified by silica gel column chromatography using a mixture of petroleum ether/ethyl acetate (20:1, v/v) as eluent to afford the desired product (0.52g, 76%) as a white solid.1H NMR (300 MHz, DMSO-d6) delta:8.96 (s, 1H, ArH), 7.89 (d, J=8.01Hz, 2H, ArH), 7.31 (m, 3H, ArH), 4.39 (q, J=7.12 Hz, 2H, -OCH2), 1.34 (t, J=7.12 Hz, 3H,-CH3).

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

Reference:
Article; Li, Zheng; Qiu, Qianqian; Xu, Xue; Wang, Xuekun; Jiao, Lei; Su, Xin; Pan, Miaobo; Huang, Wenlong; Qian, Hai; European Journal of Medicinal Chemistry; vol. 113; (2016); p. 246 – 257;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 57561-39-4, name is tert-Butyl (2-hydroxyethyl)(methyl)carbamate, 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 57561-39-4, Recommanded Product: 57561-39-4

General procedure: To a solution of tert-butyl (R)-(1-hydroxypropan-2-yl)carbamate(2a) (10.00 g, 57.1 mmol) in DCM (300 mL) was added solid Dess-Martin periodinane (33.89 g, 79.9 mmol) in one portion. Water(1.4 mL) was added dropwise within 0.5 h to the vigourously stirredsuspension, and the stirring was continued for 2 h at room temperature,whereupon EtOAc (1000 mL) was added. The suspension was filteredthrough a pad of Celite, and the filter-cake was washed with EtOAc(500 mL). Combined filtrates were washed sequentially with aqueoussaturated NaHCO3, aqueous 10% Na2S2O3 (1:1), brine, and dried(Na2SO4). Volatiles were evaporated and the residue was dried in vacuoto give aldehyde 3a as a white solid (9.30 g, 94%). 1H NMR (400 MHz,CDCl3) delta: 9.56 (s, 1H), 5.09 (m, 1H), 4.23 (qui, J=7.3 Hz, 1H), 1.45 (s,9H), 1.33 (d, J=7.3 Hz, 3H). 1H NMR spectrum was in agreement withthat reported in the literature.40

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 (2-hydroxyethyl)(methyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Cao, Sha; Gualtieri, Maxime; Hjort, Karin; Hughes, Diarmaid; Huseby, Douglas L; Ikaunieks, Martins; Katkevics, Martins; Kukosha, Tatyana; Loza, Einars; Pantel, Lucile; Racine, Emilie; Ryabova, Victoria; Sarciaux, Matthieu; Serri, Marine; Shubin, Kirill; Suna, Edgars; Trufilkina, Nadezhda; Yadav, Kavita; Bioorganic and medicinal chemistry; (2020);,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 159326-71-3, name is Pyrrolo[2,1-f][1,2,4]triazin-4(3H)-one, 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 159326-71-3, SDS of cas: 159326-71-3

A mixture of pyrrolo[2,1-f][1,2,4]triazin-4(3H)-one (14 g), DIPEA (18.1 mL), N,N-dimethylbenzeneamine (12.56 g), phosphoryl chloride (42.6 mL) and toluene (300 mL) was stirred at 100C for 12 hours. The reaction mixture was concentrated under reduced pressure. Sodium methoxide (28% in methanol solution) (140 g) was added to a suspension of the residue and THF (100 mL) at room temperature. The mixture was washed with a saturated aqueous sodium hydrogen carbonate solution at room temperature, and extracted with ethyl acetate. The organic layer was washed with a saturated brine, then dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (12.1 g). 1H NMR (300 MHz, DMSO-d6) delta 4.09 (3H, s), 6.73-6.91 (2H, m), 7.94 (1H, dd, J = 2.5, 1.6 Hz), 8.19 (1H, s).

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, Pyrrolo[2,1-f][1,2,4]triazin-4(3H)-one, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Takeda Pharmaceutical Company Limited; KAWAKITA Youichi; KOJIMA Takuto; NII Noriyuki; ITO Yoshiteru; SAKAUCHI Nobuki; BANNO Hiroshi; LIU Xin; ONO Koji; IMAMURA Keisuke; IMAMURA Shinichi; (165 pag.)EP3450436; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 60144-53-8, The chemical industry reduces the impact on the environment during synthesis 60144-53-8, name is tert-Butyl (4-fluorophenyl)carbamate, I believe this compound will play a more active role in future production and life.

To a solution of (4-fluorophenyl)-carbamic acid te/f-butyl ester (1.3 g, 6.2 mmol) in anhydrous tetrahydrofuran (15 mL) was added sodium hydride (60% dispersion in mineral oil, 261 mg, 6.8 mmol). After the initial gas evolution had ceased, the reaction was allowed to stir for 15 minutes. Tetra-n-butylammonium iodide (227 mg, 0.6 mmol) was then added followed by addition of 2-chloro-5-chloromethyl thiazole prepared above. The mixture was heated to reflux for 1 hour. After cooling, the reaction was carefully neutralized with cold saturated sodium bicarbonate (10 mL) and extracted with ethyl acetate (2 x 20 ml_). The organic layers were combined, dried over anhydrous sodium sulfate, filtered and the solvent removed under reduced pressure to provide a dark oil. Flash chromatography (silica gel; 5%-10% ethyl acetate in hexanes) provided (2-chloro-thiazol-5-ylmethyl)-(4-fluorophenyl)-carbamic acid terf-butyl ester as a yellow oil (1.5 g, 4.4 mmol).

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 (4-fluorophenyl)carbamate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; WYETH; WO2008/73461; (2008); A2;,
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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H6F3NO2S

EXAMPLE 10 Preparation of (S)-N-(tert.butoxycarbonyl)-N-propyl-6-methoxy-5-methoxycarbonyl-1,2,3,4-tetrahydro-2-naphthylamine A solution of (S)-N-(tert.butoxycarbonyl)-N-propyl-6-methoxy-5-hydroxy-1,2,3,4-tetrahydro-2-naphthylamine (1.4 g; 4.17 mmoles), prepared as described in example 9, in acetonitrile (42 ml) was added at room temperature with K2CO3 (1.15 g, 8.34 mmoles) and, dropwise, with a solution of N-phenyltrifluoromethansulfonimide (1.78 g; 5 mmoles) in acetonitrile (10 ml). The reaction mixture was heated to 55 C. for 19 hours, then the solvent was evaporated under reduced pressure. The residue was added with methylene chloride and water. The phases were separated and the organic one was washed with water, anhydrified over Na2SO4 and the solvent evaporated under reduced pressure. The residue was dissolved in dimethylsulfoxide (13 ml) and methanol (5 ml) and the solution was added, under N2 at room temperature, with triethylamine (1.1 ml, 7.87 mmoles), palladium acetate (53 mg; 0.236 mmole) and 1,3-bisdiphenylphosphinopropane (97 mg; 0.236 mmole). The reaction mixture was then heated to 70 C. under CO pressure (9 bar) for 90 hours during which further palladium acetate (18 mg, 0.080 mmole) and 1,3-bisdiphenylphosphinopropane (33 mg, 0.080 mmole) were added in one portion. After cooling to room temperature the mixture was poured into water and methylene chloride. The phases were separated and the organic one was washed with water, anhydrified over Na2SO4 and evaporated to dryness under reduced pressure. The resulting crude was purified by silica gel chromatography (eluent: petrolatum:ethyl acetate=90:10). There was obtained 1.08 g of (S)-N-(tert.butoxycarbonyl)-N-propyl-6-methoxy-5-methoxycarbonyl-1,2,3,4-tetrahydro-2-naphthylamine. 1H-NMR (200 MHz, CDCl3) delta (ppm): 0.86 (t, 3H), 1.44 (t, 9H); 1.46-2.00 (m, 4H); 2.71-3.13 (m, 6H); 3.78 (s, 3H); 3.89 (s, 3H), 3.90-4.27 (m, 1H); 6.71 (d, 1H); 7.03 (d, 1H). Mass (electronic impact): 377 (M)+

The synthetic route of 456-64-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zambon Group S.p.A.; US6232348; (2001); B1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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 17193-28-1 as follows. Safety of 1-Amino-1-cyclopentanecarboxamide

N,N-Diisopropylethylamine (0.77 mL, 4.40 mmol) was added to a solution of commercially available ((S)-5-((((9H-fluoren-9-yl)methoxy)carbonyl)amino)-2-((tert-butoxycarbonyl)amino)pentanoic acid, 4 (1 g, 2.2 mmol), 1-aminocyclopentanecarboxamide, 9 (0.282 g, 2.2 mmol) and HATU (1.255 g, 3.30 mmol) in dry acetonitrile (20 mL) at room temperature under Argon atmosphere and the resulted reaction mixture was stirred under the same conditions for 2h. The progress of the reaction was monitored by TLC. Solvent was evaporated under reduced pressure and the crude product was purified on Teledyne Isco Combiflash Rf purification machine to provide (9H-fluoren-9-yl)methyl tert-butyl (5-((1-carbamoylcyclopentyl)amino)-5-oxopentane-1,4-diyl)(S)-dicarbamate, 10 (1.18 g, 95%) as a colorless solid. ESI-MS m/z: 565.3 [M+H]+. 1H NMR (400 MHz, DMSO-d6): delta 8.02 (s, 1H, NH), 7.89 (d, J=7.4 Hz, 2H, ArH), 7.67 (d, J=7.4 Hz, 2H, ArH), 7.43-7.27 (m, 5H, ArH, NHFmoc), 7.02 (d, J=6.2 Hz, 1H, NHBoc), 6.87 (bs, 1H, CONH2), 6.85 (bs, 1H, CONH2), 4.28 (d, J=6.1 Hz, 2H, FmocCH2), 4.20 (t, J=6.8 Hz, 1H, FmocCH), 3.80 (q, J=6.8 Hz, 1H, NHCH), 2.96 (q, J=6.3 Hz, 2H, CH2NHFmoc), 2.12-1.83 (m, 4H, CH2), 1.65-1.30 (m, 17H, CH2, Boc).

According to the analysis of related databases, 17193-28-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SOUTHERN RESEARCH INSTITUTE; UAB RESEARCH FOUNDATION; Suto, Mark J.; Gupta, Vandana; Mathew, Bini; Murphy-Ullrich, Joanne; (105 pag.)US2019/127420; (2019); 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. 4141-08-6, name is 2-Amino-N-methylbenzamide, A new synthetic method of this compound is introduced below., category: amides-buliding-blocks

General procedure: To a stirred solution of 3,5-dichloro-4H-1,2,6-thiadiazin-4-one (6) (366.0 mg, 2.000 mmol) in EtOH (4 mL), at ca. 20 C, was added 5-amino-2-methylphenol (246.3 mg, 2.000 mmol) in one portion followed by 2,6-lutidine (233 muM, 4.00 mmol) and the mixture was stirred at this temperature until complete consumption of the starting material (TLC, 1 h). The yellow solid formed was then filtered under reduced pressure and washed with EtOH (2 mL), DCM (5 mL) and n-hexane (5 mL) to give the title compound 7 (477.1 mg, 77%) as orange needles

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; Asquith, Christopher R. M.; Godoi, Paulo H.; Cou ago, Rafael M.; Laitinen, Tuomo; Scott, John W.; Langendorf, Christopher G.; Oakhill, Jonathan S.; Drewry, David H.; Zuercher, William J.; Koutentis, Panayiotis A.; Willson, Timothy M.; Kalogirou, Andreas S.; Molecules; vol. 23; 5; (2018);,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics