Day: August 25, 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.110-70-3,N1,N2-Dimethylethane-1,2-diamine,as a common compound, the synthetic route is as follows.

To a stirred solution of N,N’-dimethylethylenediamine (25.0 g, 0.28 mol) in 150 mL of dry diethyl ether was added diethyl oxalate (38.5 mL, 0.28 mol) in one portion. After a few minutes white crystals started to precipitate. The reaction mixture was stirred at room temperature overnight. The product was filtered and washed with dry diethyl ether. The product was dried under vacuum at 47 C overnight to give colorless crystals (38.64 g, 96%). ?H NMR (200 MHz, CDCl3, delta) : 3.50 (s, 4H), 2.99 (s, 6H). ?3C {?H} (200 MHz, CDCI3, delta): 157.35, 45.91, 34.74.

The synthetic route of 110-70-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; GEORGIA TECH RESEARCH CORPORATION; WO2005/123754; (2005); A2;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.33527-91-2,Tris[2-(dimethylamino)ethyl]amine,as a common compound, the synthetic route is as follows.

Embodiment 5Production of [Cu(Me6tren)]BPh4 0.20 g (0.87 mmol) Me6tren (1) was dissolved in approx. 2 ml acetone and a solution of 0.30 g (0.81 mmol) [Cu(CH3CN)4]PF6 (tetrakis(acetonitrile)copper(I)-hexafluorophosphate) in approx. 4 ml acetone was added slowly under constant stirring. A solution of 0.28 g (0.82 mmol) NaBPh4 (sodium tetraphenylborate) in approx. 2 mL acetone was added subsequently to the colorless, complex solution thus obtained, for the replacement of anions. For the preparation of the solid, the complex solution was added to 20 ml diethylether. The voluminous solid of [Cu(Me6tren)]BPh4 (10) obtained was dried in vacuum. 0.48 g (96.6%) of a colorless powder was obtained as the product.All work was carried out in an argon box. It is possible, however, to carry out all work with the Schlenk technique under argon or nitrogen as well.The complex [Cu(Me6tren)]BPh4 is shown in FIG. 1.The results of the crystal structure analysis of [Cu(Me6tren)]BPh4 are shown in FIG. 2.

The synthetic route of 33527-91-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Schindler, Siegfried; Wuertele, Christian; US2012/16127; (2012); A1;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

110-70-3, N1,N2-Dimethylethane-1,2-diamine is a chiral-nitrogen-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 2-thiophenecarboxaldehyde (8.6 ml, 104 mmol) in toluene was added APatent; METABASIS THERAPEUTICS, INC.; WO2009/23718; (2009); A2;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.110-70-3,N1,N2-Dimethylethane-1,2-diamine,as a common compound, the synthetic route is as follows.

Example 20Preparation of (E)-methyl 4-(methyl(2-((4Z,7Z,10Z,13Z,16Z,19Z)-N-methyldocosa-4,7,10,13,16,19-hexaenamido)ethyl)amino)-4-oxobut-2-enoate (Compound I-104) tert-Butyl methyl(2-(methylamino)ethyl)carbamate was prepared as follows: N1,N2-dimethylethane-1,2-diamine (40 mmol) was dissolved in 100 mL of CH2Cl2 and cooled to 0 C. A solution of di-tert-butylcarbonate (4.0 mmol) in CH2Cl2 (10 mL) was then added dropwise at 0 C. over a period of 15 min. The resulting reaction mixture was stirred at 0 C. for 30 min and then warmed to room temperature. After stirring at room temperature for 2 h, the reaction mixture was diluted with CH2Cl2 (100 mL). The organic layer was washed with brine (3¡Á25 mL), dried (Na2SO4) and concentrated under reduced pressure to afford tert-butyl methyl(2-(methylamino)ethyl)carbamate. This amine was subjected to the same reaction conditions outlined earlier in the preparation of (E)-methyl 4-(2-(4Z,7Z,10Z,13Z,16Z,19Z)-docosa-4,7,10,13,16,19-hexaenamidoethylamino)-4-oxobut-2-enoate. The desired product, namely (E)-methyl 4-(methyl(2-((4Z,7Z,10Z,13Z,16Z,19Z)-N-methyldocosa-4,7,10,13,16,19-hexaenamido)ethyl)amino)-4-oxobut-2-enoate, was obtained after purification by silica gel chromatography. MS (EI) calcd for C31H46N2O4: 510.35. found 511 (M+1).

As the paragraph descriping shows that 110-70-3 is playing an increasingly important role.

Reference£º
Patent; Milne, Jill C.; Jirousek, Michael R.; Bemis, Jean E.; Vu, Chi B.; US2011/172240; (2011); A1;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

119139-23-0, 3,4-Di(1H-indol-3-yl)-1H-pyrrole-2,5-dione is a chiral-nitrogen-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A reaction flask equipped with a magnetic stirrer was charged with a solution of 3, 4-bisindolylmaleimide (2.1 g, 6.4 mmol) in 100 mL of acetone. Potassium hydroxide (0.40 g, 7.1 mmol) was added to the solution at 0 C and stirred for 0.5 h. Iodomethane (1.6 g, 0.011 mol) or 1-bromooctane (2.4 g, 0.012 mol) was added to the reaction mixture for 3, 4-bisindolyl-1-N-methylmaleimide or 3, 4-bisindolyl-1-N-(n-octyl)maleimide, respectively. The reaction mixture was warmed to room temperature and stirred for 1 h (iodomethane) or 24 h (1-bromooctane). The reaction mixture was concentrated and then dissolved in a mixture of ethyl acetate and water. The organic phase was separated, washed with water once and brine once, dried over anhydrous sodium sulfate. The product was purified by flash chromatography with petroleum ether, ethyl acetate and dichloromethane (V/V = 3:1:2) as eluent.

119139-23-0 3,4-Di(1H-indol-3-yl)-1H-pyrrole-2,5-dione 2399, achiral-nitrogen-ligands compound, is more and more widely used in various.

Reference£º
Article; Zhang, Qianfeng; Chang, Guanjun; Zhang, Lin; Chinese Chemical Letters; vol. 29; 3; (2018); p. 513 – 516;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

31886-58-5, (R)-(+)-N,N-Dimethyl-1-ferrocenylethylamine is a chiral-nitrogen-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example B18: Reaction schemeX24 ml (10 mmol) of n-BuLi (2.5 M in hexane) are added dropwise to a solution of 3.44 g (10 mmol) of 1 ,1 ‘-dibromoferrocene in 10 ml of tetrahydrofuran (THF) at a temperature of < -30C. The mixture is stirred at this temperature for a further 1.5 hours. 2.21 ml (10 mmol) of dicyclohexylphosphine chloride are then added dropwise at such a rate that the temperature does not exceed -20C. After stirring the mixture for a further 10 minutes, the temperature is allowed to rise to room temperature and the mixture is stirred for another one hour. It is cooled back down to 30C and 4.4 ml (11 mmol) of n-BuLi (2.5 M in hexane) are added dropwise. The mixture is subsequently stirred at -10C for 30 minutes. The reaction mixture is then cooled to -78C and 1.49 ml (11 mmol) of dichlorophenylphosphine are added. The mixture is stirred at -78C for 20 minutes and then at room temperature for a further one hour. This gives a reaction mixture comprising the monochlorodiphosphine X6. In a second vessel, 8.5 ml (11 mmol) of S-BuLi (1.3 M in cyclohexane) are added dropwise to a solution of 2.57 g (10 mmol) of (R)-1-dimethylamino-1-ferrocenylethane in 15 ml of diethyl ether at <-10C. After stirring the mixture at the same temperature for 10 minutes, the temperature is allowed to rise to 0C and the mixture is stirred for another 1.5 hours. This reaction solution is subsequently added by means of a cannula to the reaction mixture comprising the monochlorodiphosphine X6 which has been cooled to -10C. After the addition, the mixture is stirred at room temperature for another 2 hours. After addition of 10 ml of water, the reaction mixture is extracted, the organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure on a rotary evaporator. The residue is heated at 140C for one hour. Column chromatography (silica gel 60; eluent: hexane/ethyl acetate 4:1 ) gives the compound of the formula (B1 ) in a yield of 47%. 31P- and 1H-NMR of the product are identical with those of Example B1.; Example B19: Reaction schemeReaction mixture 1 : 4 ml (10 mmol) of n-BuLi (2.5 M in hexane) are added dropwise to a solution of 3.44 g (10 mmol) of 1 ,1 '-dibromoferrocene in 10 ml of tetrahydrofuran (THF) at a temperature of < -30C. The mixture is stirred at this temperature for a further 30 minutes. It is then cooled to -78C and 1.36 ml (10 mmol) of phenyldichlorophosphine are added. After stirring the mixture for a further 10 minutes, the temperature is allowed to rise to room temperature and the mixture is stirred for another one hour.Reaction mixture 2: In a second vessel, 8.0 ml (10.4 mmol) of S-BuLi (1.3 M in cyclohexane) are added dropwise to a solution of 2.57 g (10 mmol) of (R)-1-dimethylamino-1-ferrocenyl- ethane in 15 ml of diethyl ether at <-10C. After stirring the mixture at the same temperature for 10 minutes, the temperature is allowed to rise to 0C and the mixture is stirred for another 1.5 hours.The reaction mixture 1 is slowly added to the reaction mixture 2 at a temperature below -10C. The mixture is subsequently stirred at room temperature for 1.5 hours. At a temperature in the range from -78C to -50C, 8 ml (10.4 mmol) of S-BuLi (1.3 M in cyclohexane) are then added dropwise. After stirring the mixture at -78C for 20 minutes, the temperature is allowed to rise to 0C and the mixture is stirred for a further 30 minutes before 2.21 ml (10 mmol) of chloro- dicyclohexylphosphine are added at -20C. The mixture is stirred at 20C for another 20 minutes and finally at room temperature for another 1.5 hours. The work-up and thermal epimerization are carried out in a manner analogous to that described in Example B18. The compound of the formula (B1 ) is obtained in a yield of 31 %. 31P- and 1H-NMR of the product are identical with those of Example B1.; Example B20:8.5 ml (11 mmol) of S-BuLi (1.3 M in cyclohexane) are added dropwise to a solution of 2.83 g (1 1 mmol) of (R)-1 -dimethylamino-1 -ferrocenylethane in 15 ml of diethyl ether at <-10C. The cooling is then removed and the mixture is stirred at room temperature for another 2 hours. After cooling to -10C, 2.92 g (10 mmol) of the compound A3 are added and the mixture is stirred at this temperature for a further 30 minutes. The temperature is allowed to rise to room temperature and the mixture is stirred for another one hour. After addition of 10 ml of 1 N NaOH, the reaction mixture is extracted, the organic phase is dried over sodium sulphate and the solvent is distilled off under reduced pressure on a rotary evaporator. A 1H-NMR of the residue shows that the reaction is very stereoselective and gives virtually exclusively the desired diastereomer (RC,SFC, Sp)-I -[2-(1 -dimethylaminoethyl)ferrocen-1 -yl]phenylphosphino- 1 '-dicyclohexylphosphinoferrocene. After chromatography (silica gel 60; eluent = hexane/ethyl acetate 4:1 ), this product is obtained in a yield of 37%. 31P- and 1H-NMR of the produ…

As the paragraph descriping shows that 31886-58-5 is playing an increasingly important role.

Reference£º
Patent; SOLVIAS AG; WO2007/116081; (2007); A1;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.33527-91-2,Tris[2-(dimethylamino)ethyl]amine,as a common compound, the synthetic route is as follows.

To a solution of tris(2-dimethylaminoethyl)amine (0.401 g, 1.74 mmol) in acetonitrile (4 mL) was added 1-bromododecane (1.34 g, 5.38 mmol). The resulting mixture was heated at reflux with stirring for 22 hours, during which time awhite solid was observed. After cooling, and the addition of a cold hexanes/acetone mixture (15 mL, 1:1), to the reaction flask, the precipitate was filtered with a Buchner funnel, and rinsed with a cold hexanes/acetone mixture (20 mL, 1:1), resulting in T-12,12,12 (1.39 g, 82%) as a white powder; mp=225-254 C; ?H NMR (300 JVII-Tz, CDC13) oe 4.11-4.03 (m, 6H), 3.63-3.55 (m, 6H), 3.39-3.32 (m, 6H), 3.30(s, 18H), 1.72-1.62 (m, 6H), 1.37-1.14 (m, 54H), 0.84-0.78 (m, 9H); ?3C NMR (75 MHz, CD3OD) 3 65.3, 61.0, 50.1, 46.8, 31.7, 29.4, 29.3, 29.3, 29.1, 29.0, 26.1, 22.4, 22.4, 13.1; high resolution mass spectrum (ESI) m/z 245.9435 ([Mj3 calculated for [C48H,o5N4j3: 245.9441). See also Yoshimura et al., 2012, Langmuir 28:9322-933 1. ?H and ?3C NMR spectra of compound T-12,12,12 can be found in Figure 52.

33527-91-2 Tris[2-(dimethylamino)ethyl]amine 263094, achiral-nitrogen-ligands compound, is more and more widely used in various.

Reference£º
Patent; TEMPLE UNIVERSITY-OF THE COMMONWEALTH SYSTEM OF HIGHER EDUCATION; VILLANOVA UNIVERSITY; WUEST, William, M.; MINBIOLE, Kevin, P.C.; BARBAY, Deanna, L.; (227 pag.)WO2016/172436; (2016); A1;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.31886-58-5,(R)-(+)-N,N-Dimethyl-1-ferrocenylethylamine,as a common compound, the synthetic route is as follows.

6.0g (R) -1- ferrocenyl ethyldimethylamine was added 20mL of dry tert-butyl methyl ether, in an ice bath, under an argon atmosphere was slowly added dropwise 21.5mL 1.3mol / L tert-butyllithium n-hexane solution, warmed to room temperature after dropwise addition, reaction was stirred for 1 hour and then added dropwise dissolved in 20mL of MTBE to the reaction solution at -78 deg.] C 5.52g of p-toluenesulfonyl azide, after the reaction at -78 5 h, slowly warmed to 0 deg.] C, stirred for 10 minutes, dissolved in 250mL of distilled water was added 11.6g of sodium pyrophosphate decahydrate, stirred at room temperature overnight, the reaction was stopped extracted with dichloromethane (3 ¡Á 80mL), the organic layer was dried over anhydrous magnesium sulfate, and rotary evaporation to obtain a reddish black oil, separated by column chromatography (eluent volume of ethyl acetate and triethylamine as the 30: 1 mixture, silica gel 300 to 400 mesh), to give a red-brown oil azide 5.7g, yield of 82%.

The synthetic route of 31886-58-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Shaanxi Normal University; Chai Yonghai; Ren Xiaochen; He Chunyan; Chen Weiping; Zhang Shengyong; (14 pag.)CN104592313; (2017); B;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.110-70-3,N1,N2-Dimethylethane-1,2-diamine,as a common compound, the synthetic route is as follows.

36.2 g (0.40 mol) acrylic acid chloride and 16 mg MEHQ were dissolved in 600 ml methylene chloride in a 1.5-l sulphonation flask and cooled to -5 C. Then, a mixture of 17.6 g (0.20 mol) N,N’-dimethylethylenediamine, 40.8 g (0.40 mol) triethylamine and 400 ml methylene chloride was added dropwise accompanied by stirring so that the temperature remained between -5 and 0 C. After 1.5 h stirring, the mixture was allowed to warm up to room temperature, stirred overnight, the precipitate formed was filtered off and the filtrate concentrated under vacuum. The raw product was taken up in 150 ml acetone, filtered through a frit with 50 g silica gel 60 and concentrated again. After repeating this process, 30.1 g (77% yield) of a light yellow liquid remained. 1H-NMR (400 MHz, CDCl3): delta=3.10 and 3.14 (s; 2*3H, CH3), 3.54-3.67 (2m; 4H, CH2N), 5.68, 6.35 and 6.56 (m; 3*2H, CH=CH2) ppm.

110-70-3 N1,N2-Dimethylethane-1,2-diamine 8070, achiral-nitrogen-ligands compound, is more and more widely used in various.

Reference£º
Patent; Ivoclar Vivadent AG; US6953832; (2005); B2;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.110-70-3,N1,N2-Dimethylethane-1,2-diamine,as a common compound, the synthetic route is as follows.

To a solution of N,N’-dimethylethylenediamine (300 mg) in DMF (2.0 mL) was added K2CO3 (1.0 g) and compound B (466 mg). The mixture was heated at 80C for 3h. Solvent was evaporated and the residue was extracted with DCM and then purified by a prep-TLC plate (10%MeOH/DCM with 1% NH3 in methanol) to give product as a yellow solid (400 mg, yield 75%).

As the paragraph descriping shows that 110-70-3 is playing an increasingly important role.

Reference£º
Patent; ARIAD PHARMACEUTICALS, INC.; ZHU, Xiaotian; WANG, Yihan; SHAKESPEARE, William, C.; HUANG, Wei-Sheng; DALGARNO, David, C.; WO2013/169401; (2013); A1;,
Chiral nitrogen ligands in late transition metal-catalysed asymmetric synthesis¡ªI. Addressing the problem of ligand lability in rhodium-catalysed hydrosilations
Nitrogen-Containing Ligands for Asymmetric Homogeneous and Heterogeneous Catalysis