Tag: M.W=200-300

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. 118684-31-4, name is tert-Butyl (3-(hydroxymethyl)phenyl)carbamate, A new synthetic method of this compound is introduced below., category: amides-buliding-blocks

Comp nd 14B: tert-but l 3-form l hen l carbamate Compound 14A (13.8 g, 61.81 mmol, 1.00 equiv) was dissolved in DCE (400 mL) and Mn02 (54 g, 621.14 mmol, 10.05 equiv) was then added. The mixture was left under agitation at ambient temperature for 3 days after which the solids were removed by filtering. The filtrate was evaporated to dryness and the residue was purified on a silica column with a mixture of EtOAc and PE (1 :30) to yield 3 g (22 %) of compound 14B in the form of a white 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; PIERRE FABRE MEDICAMENT; RILATT, Ian; PEREZ, Michel; GOETSCH, Liliane; BROUSSAS, Matthieu; BEAU-LARVOR, Charlotte; HAEUW, Jean-Francois; WO2015/162293; (2015); A1;,
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Synthetic Route of 6292-59-7, 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. 6292-59-7, name is 4-(tert-Butyl)benzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of p-tert-butylbenzenesulfonamide (VI) (13.5 g, 63 mmol) was dissolved in sodium hydroxide solution (31.5 mL, 2N) and the solvent was distilled off under reduced pressure to give the sodium salt of p-tert-butylbenzenesulfonamide.A solution of tert-butylbenzenesulfonamide sodium and 4,6-dichloro-5- (2-methoxyphenoxy) -2,2 ‘-bipyridine (V) (21.05 g, 60.3 mmol) (200 mL) and heated to 90 ° C with stirring for 3 h. TLC was complete. The residue was diluted with IN hydrochloric acid and the pH was adjusted to 3 to 4 with IN hydrochloric acid. The crystals were recrystallized and dried under reduced pressure to give 29.5 g of a white solid as N- [6-chloro (2-methoxyphenoxy) [2,2 ‘] – dipyridyl] -4-yl] -4- (1,1-dimethylethyl) -benzenesulfonamide (W) The yield was 93percent.

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, 4-(tert-Butyl)benzenesulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shanghai Tianci International Pharmaceutical Co., Ltd.; Li Xinjuanzi; Li Jianzhi; Ma Xilai; Chi Wangzhou; Liu Hai; Hu Xuhua; Zheng Xiaoli; Zhai Zhijun; Li Jianxun; (14 pag.)CN104193687; (2017); B;,
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Some common heterocyclic compound, 127-77-5, name is 4-Amino-N-phenylbenzenesulfonamide, molecular formula is C12H12N2O2S, 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: 4-Amino-N-phenylbenzenesulfonamide

Triethylamine (0.07 mL, 0.5 mmol) and phenyl isothiocyanate (2.1 mL, 11 mmol) were added sequentially to a solution of 4 (2.48 g, 10 mmol) in dry THF (10 mL). After heating under reflux for 48 h, all volatiles were removed under vacuum, and the resulting crude material was purified by flash chromatography on silica gel (hexanes/acetone, 3:1) to afford N-phenyl-4-[[(phenylamino)thioxomethyl]amino]benzenesulfonamide (5, also called LED209) (1.34 g, 35%) as a white solid, mp 160-162C. 1H NMR (CD3COCD3, 300 MHz) delta 9.35 (br s, 1H), 9.30 (br s, 1H), 8.98 (br s, 1H), 7.80-7.72 (m, 4H), 7.51-7.47 (m, 2H), 7.38-7.33 (m, 2H), 7.28-7.16 (m, 5H), 7.08-7.04 (m, 1H); 13C NMR (CD3COCD3, 75 MHz) delta 180.2, 143.9, 138.9, 138.2, 135.2, 129.3 (2C), 129.1 (2C), 127.9 (2C), 125.8, 124.6 (3C), 122.8 (2C), 120.8 (2C). Compound 27 was prepared in a similar manner as compound 3 in 90% yield; 1H NMR (CD3COCD3, 300 MHz) delta 9.63 (br s, 1H), 7.80-7.77 (m, 2H), 7.46-7.42 (m, 2H), 7.35-7.27 (m, 3H), 7.15-7.12 (m, 2H), 3.17 (s, 3H), 2.14 (s, 3H). Compound 8 was prepared in a similar manner as compound 4 in 65% yield; 1H NMR (CD3COCD3, 300 MHz) delta7.32-7.13 (m, 7H), 6.68-6.65 (m, 2H), 5.53 (br s, 2H), 3.10 (s, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 127-77-5, its application will become more common.

Reference:
Patent; The Board of Regents of The University of Texas System; Omm Scientific, Inc.; SPERANDIO, Vanessa; FALCK, John R.; STEWART, Donald R.; (96 pag.)EP2219635; (2017); B1;,
Amide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 6292-59-7, name is 4-(tert-Butyl)benzenesulfonamide, 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 6292-59-7, Safety of 4-(tert-Butyl)benzenesulfonamide

p-t-butyl benzene sulphonamide (2.2 g, 0.0104 mol) was taken in Dimethyl Sulphoxide and potassium carbonate was added (2.75 g, 0.0198 mol) under inter atmosphere and stirred for 0.5 h. 3.4 g of 4,6- dichloro 5-(2-methoxyphenoxy) [2,2]-bipyrimidinyl compound (formula-3) 3.44 g, 0.009 mol was added and heated to 120° C. and maintained at the same temperature for 2 h. The reaction mass was quenched in iN hydrochloric acid and stirred for 2 h. Product precipitates out and was filtered and washed with water and dried under vacuum yielding 4.3 g (9 6percent) of pale yellow crystalline solid 4,6- dichioro 5-(2-methoxyphenoxy) [2,2]- bipyrimidinyl compound of formula-3 having the X-ray diffraction pattern with peaks at 8.547, 9.867, 11.068, 11.97, 13.851, 14.726, 15.539, 17.213, 18.428, 20.463, 22.232, 22.704, 23.536,23.937, 24.827, 26.291, 26.545, 27.294, 27.815, 28.223,29.278, 30.022, 30.5, 31.447, 31.996, 32.454, 33.43, 33.644,34.251, 34.89, 35.662, 36.393, 37.402, 38.523, 39.022,40.238, 40.724, 41.35, 41.93, 43.732, 44.289, 45.24, 47.267, 47.978,49.123,49.438, 50.22, ±0.2 degrees two theta values.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Biocon Limited; Venkata, Srinivas Pullela; Kothakonda, Kiran Kumar; Rajmahendra, Shanmughasamy; Chandrasekaran, Indrajit; Kaliappan, Mariappan; Mailar, Rekha Shivappa; US2014/275535; (2014); A1;,
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Reference of 4793-24-2,Some common heterocyclic compound, 4793-24-2, name is 2-Chloro-4-fluoro-5-sulfamoylbenzoic acid, molecular formula is C7H5ClFNO4S, 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 a solution of 2-chloro-4-fluoro-5-sulfamoylbenzoic acid (3.2 g, 12.65 mmol) in THF (10 mL) was added IM BH3 THF (38 mL, 38.0 mmol). After stirring 12h, the reaction mixture was quenched with MeOH and concentrated in vacuo. The residue was purified by chromatography (silica, EtO Ac-Hex) to afford 4-chloro-2-fluoro-5- (hydroxymethyl)benzenesulfonamide (1.9 g). To a suspension of 4-chloro-2-fluoro-5- (hydroxymethyl)benzenesulfonamide (1.78 g, 7.43 mmol) in DCM (10 mL) was added PBr3 (2.2 Ig, 8.17 mmol). The reaction was stirred for 24 h when it was determined to be complete by GCMS. The reaction was carefully quenched with H2O and then partitioned between THF and brine. The organic layer was dried over Na2SO4 and concentrated in vacuo to afford 5-(bromomethyl)-4-chloro-2-fluorobenzenesulfonamide (1.98 g) as an off-white solid. 1H-NMR (DMSO-J6, 400 MHz) delta 8.08 (d, J = 7.8 Hz, IH), 7.84 (s, 2H), 7.80 (d, J = 9.9 Hz, IH), 4.83 (s, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-4-fluoro-5-sulfamoylbenzoic acid, its application will become more common.

Reference:
Patent; EXELIXIS, INC.; BOLLU, Venkataiah; BOREN, Brant, Clayton; DALGARD, Jackline, Eve; FLATT, Brenton, T.; HAQ, Nadia; HUDSON, Sarah; MOHAN, Raju; MORRISSEY, Michael; PRATT, Benjamin; WANG, Tie-lin; WO2010/93845; (2010); 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. 456-64-4, name is 1,1,1-Trifluoro-N-phenylmethanesulfonamide, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1,1,1-Trifluoro-N-phenylmethanesulfonamide

tert-Butyl 4-{ [(trifluoromethyl)sulfonyl] oxy}-3,6-dihydropyridine-l(2H)-carboxylateDi-wo-propylamine (22 ml) was dissolved in dry THF (125 ml) and cooled to -78C. «-Butyllithium (62.5 ml, 2.5M) was added dropwise. The solution was stirred for 15 minutes, then tert-bntyl 4-oxopiperidine-l-carboxylate (28.32 g) in THF (100 ml) was added dropwise. The reaction mixture was stirred for 1 hour at -78C, then N- phenyltrifluoromethanesulfonimide (53.8 g) in THF (150 ml) was added dropwise. The reaction mixture was stirred at -78C for 2 hours and allowed to warm up to room temperature and stirred overnight. The reaction mixture was then concentrated in vacuo and the residue dissolved in ether (1000 ml). This was washed with water (500 ml), 2M sodium hydroxide solution (3 x 500 ml), water (500 ml) and brine (500 ml) then dried over magnesium sulfate and concentrated to give the title compound as a pale brown oil (45.38 g, 96%) which was used without further purification; 1H NMR (CDCl3) deltal.48 (9H, s), 2.44 (2H, m), 3.63 (2H, t), 4.00 (2H, q), 5.70 (IH, br m).

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 456-64-4.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2007/60408; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 744183-20-8, The chemical industry reduces the impact on the environment during synthesis 744183-20-8, name is tert-Butyl exo-3-amino-8-azabicyclo[3.2.1]octane-8-carboxylate, I believe this compound will play a more active role in future production and life.

To a mixture of the product of the previous step (1020 mg, 3.42 mmol) and tert25 butyl (1R,3s,55)-3-amino-8-azabicyclo[3.2.ljoctane-8-carboxylate (774 mg, 3.42 mmol)in DMSO (34.3 mL) was added DIPEA (1.787 mL, 10.26 mmol) at RT. The resultingmixture was stirred at 120 C for 19 h. Solvent was removed by rotary evaporation to give cmde product, which was purified by column chromatography to give the titlecompound as a brown solid (513 mg, 30.7% yield). (m/z): [M+Hj calcd for C25H34C1N503 488.24 found 488.2.

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 exo-3-amino-8-azabicyclo[3.2.1]octane-8-carboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THERAVANCE BIOPHARMA R&D IP, LLC; HUDSON, Ryan; KOZAK, Jennifer; FATHEREE, Paul R.; PODESTO, Dante D.; BRANDT, Gary E.L.; FLEURY, Melissa; BEAUSOLEIL, Anne-Marie; HUANG, Xiaojun; THALLADI, Venkat R.; (121 pag.)WO2016/191524; (2016); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 2618-96-4, name is Dibenzenesulfonimide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C12H11NO4S2

General procedure: Under N2, ynamide 1a (0.300 mmol, 108.7 mg) and diphenylsulfonimide (2a; 0.600 mmol, 178.4 mg, 2.00 equiv) were dissolved in CH2Cl2 (4.00 mL). The reaction mixture was allowed to stir at r.t. After the consumption of 1a (4.5 h, TLC, eluent: PE-EtOAc, 4:1), the mixture was concentrated, and the residue was purified by flash chromatography on silica gel (eluent: PE-EtOAc, 6:1 ? 4:1) to afford 3a.

The synthetic route of 2618-96-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yu, Lian; Deng, Yuan; Cao, Jian; Synthesis; vol. 47; 6; (2015); p. 783 – 788;,
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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. 51-06-9, name is 4-Amino-N-(2-diethylaminoethyl)benzamide, A new synthetic method of this compound is introduced below., category: amides-buliding-blocks

Reactions were carried out by the oxidation of PAH by DPCfollowed under pseudo first order conditions where [PAH] [DPC] in both uncatalyzed and ruthenium(III) catalyzed(10 fold excess) reactions at room temperature. The kineticreactions and measurements were followed by our previouslab work.[5] UV-vis spectral changes observed during the oxidationreaction in the absence and presence of Ru(III) wasshown in (Figure S1). In the both cases the pseudo-first orderrate constants (kU and kC) were obtained from the plots oflog(Absorbance) versus time (Figure S1). The pseudo-firstorder plots were linear over three half-lives. The rate constants,kU and kC values are shown in Tables 1 and 2. As theFigure 1 shows that the spectral changes observed during bothuncatalyzed and catalyzed reactions at standard condition.From Figure 1 the concentration of DPC decreases slowly at415 nm. During the kinetics, a constant concentration viz.5.0105 mol dm3 of KIO4 was used throughout the study.

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; Meti, Manjunath D.; Nandibewoor, Sharanappa T.; Chimatadar, Shivamurti A.; Inorganic and Nano-Metal Chemistry; vol. 50; 4; (2020); p. 195 – 204;,
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Synthetic Route of 207405-68-3, A common heterocyclic compound, 207405-68-3, name is tert-Butyl endo-3-amino-8-azabicyclo[3.2.1]octane-8-carboxylate, molecular formula is C12H22N2O2, 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.

General procedure: To the solution of compound 8 (0.23g, 1.2mmol) in THF (5mL) was added DIPEA (1.8mmol) and bicyclic amine or piperidin amine (1.44mmol). The reaction was stirred at r.t. for overnight. Then the mixture was diluted with ethyl acetate, washed with brine, dried over MgSO4, and evaporated. The residue was purified by column chromatography to give the product. 4.1.4 40 tert-butyl 4-((2-chloro-6, 7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)amino)piperidine-1-carboxylate (9)

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; Fang, Yuanying; Xiong, Lijuan; Hu, Jianguo; Zhang, Shaokun; Xie, Saisai; Tu, Liangxing; Wan, Yang; Jin, Yi; Li, Xiang; Hu, Shaojie; Yang, Zunhua; Bioorganic Chemistry; vol. 86; (2019); p. 103 – 111;,
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Amide – an overview | ScienceDirect Topics