Month: August 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.

General procedure: To a cooled to 0 C suspension consisting of N,N’-dimethyl-1,2-ethylenediamine (4.4 g, 0.05 mol), sodium bicarbonate (33.6 g, 0.40 mol), and CH2Cl2 (50 mL), a solution of 2-bromopropionyl chloride (1a) (25.7 g, 0.15 mol) in CH2Cl2 (40 mL) was added. The reaction temperature was maintained within 0-5 C and the addition time was 40 min. The mixture was stirred for 4 h at the same temperature. Water (130 mL) and CH2Cl2 (60 mL) were added and the organic layer was separated. The combined organic fractions were dried over sodium sulfate. The solvent was removed under reduced pressure. The residue was treated with hexane (30 mL) and a solid product was filtered off and recrystallized from diethyl ether to give pure compound 2a (13.25 g, 74%), m.p. 77.0-77.4 C (from diethyl ether).

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

Reference£º
Article; Goncharova; Yakushchenko; Raevskaya; Yakushchenko; Konovalova; Russian Chemical Bulletin; vol. 68; 1; (2019); p. 181 – 185; Izv. Akad. Nauk, Ser. Khim.; 1; (2019); p. 181 – 185,5;,
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

33527-91-2, Tris[2-(dimethylamino)ethyl]amine is a chiral-nitrogen-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of tris(2-dimethylaminoethyl)amine (0.486 g, 2.11 mmol) in acetonitrile (4 mL) was added 1-bromoundecane (1.55 g, 6.57 mmol). The resulting mixture was heated at reflux with stirring for 19 hours. After cooling, and the addition of hexanes (5 mL), a white solid precipitated, which was filtered with aBuchner funnel, transferring with a cold hexanes/acetone mixture (15 mL, 1:1). The solid was rinsed with a cold hexanes/acetone mixture (2O mL, 1:1), resulting in T11,11,11 (1.62 g, 82%) as a white powder; mp=224-253 C; ?H NMR (300 MHz, CDC13) oe 4. 12-4.03 (m, 6H), 3.65-3.56 (m, 6H), 3.45-3.37 (m, 6H), 3.34 (s, 18H), 1.79-1.66 (m, 6H), 1.41-1.18 (m, 48H), 0.89-0.82 (m, 9H); ?3C NMR (75 MHz,CD3OD) oe 65.4, 61.1, 50.1, 46.9, 31.6, 29.3, 29.3, 29.2, 29.0, 28.9, 26.1, 22.4, 22.3,13.0; high resolution mass spectmm (ESI) m/z 231.9281 ([Mj3 calculated for [C45H99N4j3: 231.9284). ?H and ?3C NMR spectra of compound T-11,11,11 can be found in Figure 51.

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

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.110-70-3,N1,N2-Dimethylethane-1,2-diamine,as a common compound, the synthetic route is as follows.

The compound N,N’-dimethylethylenediamine (20 g, 0.226 mol)Soluble in 100mL of dichloromethane,50 mL of Boc anhydride (14.8 g, 0.068 mol) was added dropwise in an ice water bath.Dichloromethane mixture,Drop the room temperature reaction,The progress of the reaction was monitored by TLC (DCM: MeOH = 10:1). filter,The dry filtrate was concentrated under reduced pressure at 40 C.After the column, the product was 9g.

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

Reference£º
Patent; Sichuan Bai Li Pharmaceutical Co., Ltd.; Zhu Yi; Li Jie; Wan Weili; Zhuo Shi; Li Gangrui; (28 pag.)CN109106951; (2019); A;,
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

The above mentioned protocol was adapted for preparation ofligand L2. In a solution of 2-(chloromethyl)-3,4-dimethoxypyridinehydrochloride (2.09 g, 9.34 mmol) in 10 mL of water, a solution ofpotassium bicarbonate(2.73 g, 19.74 mmol) in water (10 mL) wasadded dropwise. The reaction mixture was stirred at room temperaturefor next 30 min. After stirring is done, solution was extractedwith dichloromethane (3 20 mL). The combined dichloromethanelayer was treated with anhydrous sodium sulfate. Thesolution was filtered and solvent was removed by rotatory evaporation.The collected light yellow oil was dissolved in dichloromethane(10 mL). The 2-(chloromethyl)-3,4-dimethoxypyridinesolution in dichloromethane was added dropwise to a solution of N,N0-dimethylethylenediamine (0.503 mL, 4.67 mmol) in dichloromethane(15 mL). In the next step aqueous 1 M sodium hydroxide(10 mL) was slowly added and solution was stirred for additional60 h at room temperature. After 60 h of stirring followed by therapid addition of a second fraction of aqueous 1 M sodium hydroxide(10 mL, 10 mmol), the product was extracted with dichloromethane(3 25 mL). The combined organic layers were driedover anhydrous sodium sulfate and filtered. Subsequently, theexcess solvent was evaporated by vacuum to afford yellow colorviscous oil (1.86 g, Yield 89%). 1H NMR (500 MHz, Methanol-d4) d8.14 (d, 2H, pyridine ring), 7.05 (d, 2H, pyridine ring), 3.95 (s,6H,-O-CH3-Py), 3.85 (s, 6H,-O-CH3-Py), 3.66 (s, 4H,-N-CH2-Py),2.67 (s, 4H, -CH2-CH2-), 2.26 (s, 6H, -N-CH3). 13C NMR (126 MHz,Methanol-d4) d 160.77, 152.19, 147.28, 146.07 (d, J = 10.3 Hz),108.87, 61.40, 58.17, 56.43, 56.07, 43.10. ESI-MS (in CH3OH).observed m/z 391.3 [(L2 + H)+] (z = 1); theoretical-391.23[(L2 + H)+] (z = 1). IR (cm1): 3375, 2945, 1626, 1584, 1447, 1425,1261, 1228, 1173, 1073, 994, 828, 651, 603.

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

Reference£º
Article; Singh, Nirupama; Niklas, Jens; Poluektov, Oleg; Van Heuvelen, Katherine M.; Mukherjee, Anusree; Inorganica Chimica Acta; vol. 455; (2017); p. 221 – 230;,
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

(S)-Ugi-amine 1 (2.57 g, 10 mmol) was dissolved in 25 mL of diethyl ether, and n-butyllithium (8 mL, 2.5 mol/L) was added dropwise to the reaction system under nitrogen protection and ice salt bath cooling. After that, the temperature was slowly raised to room temperature, and the reaction was stirred for 3 hours. Under ice cooling, chlorobis(3,5-dimethylphenyl)phosphine (5.53 g, 20 mmol) was added dropwise thereto, and after the completion of the dropwise addition, the mixture was slowly warmed to room temperature, and the reaction was stirred for 24 hours. The reaction was quenched with saturated sodium bicarbonate solution and extracted with dichloromethane. Dry over anhydrous sodium sulfate, Concentration and column chromatography gave the product 10 (3.03 g, 61%).

31886-58-5 (R)-(+)-N,N-Dimethyl-1-ferrocenylethylamine 16212257, achiral-nitrogen-ligands compound, is more and more widely used in various.

Reference£º
Patent; Zhejiang University of Technology; Zhong Weihui; Ling Fei; Nian Sanfei; (14 pag.)CN108774271; (2018); A;,
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

15.4 ml of a cyclohexane solution of s-butyllithium (1.3 M, 22 mmol) are added to a solution of 5.14 g (20 mmol) of (R)-N, N-dimethyl-1 -ferrocenylethylamine [(R)-ugi- amine] in 30 ml of t-butyl methyl ether (TBME) at <20C over a period of 10 minutes. The mixture is then heated to 00C while stirring and maintained at this temperature for 1.5 hours. It is then cooled to <60C and 3.0 ml (20 mmol) of dichlorocyclohexyl- phosphine are added over a period of 10 minutes. After stirring at -78C for30 minutes, the mixture is allowed to warm slowly to room temperature and is stirred at this temperature for 1.5 hours. 31886-58-5 (R)-(+)-N,N-Dimethyl-1-ferrocenylethylamine 16212257, achiral-nitrogen-ligands compound, is more and more widely used in various. Reference£º
Patent; SOLVIAS AG; WO2008/55942; (2008); 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.

(1) Raw material storage tanks 1,4 are respectively methyl tert-butyl ether solution of N,N-dimethyl-(R)-1-[(S)-ferrocenyl]ethylamine (mass fraction 15%) And n-hexane solution of n-butyllithium (2.7M), methyl t-butyl group of N,N-dimethyl-(R)-1-[(S)-ferrocenyl]ethylamine was controlled by a metering pump the flow rate of the ether solution was 50 mL/min, the flow rate of the n-hexane solution of n-butyllithium was 14 mL/min, and the thermostatic module injected into the microchannel reactor was thermostated at 25 C; after constant temperature treatment, the first mixing module of the microchannel reactor was introduced. The reaction was carried out at a reaction temperature of 25 C and a residence time of 10.7 s.(2) reacting the effluent of the first mixing module with diphenylphosphine chloride in a second mixing module, controlling the flow rate of diphenylphosphonium chloride to 7 mL/min by a metering pump, and the reaction temperature is 35 C, and residence time 9.8s.(3) The effluent of the microchannel reactor was acidified to neutral with concentrated hydrochloric acid, extracted with ethyl acetate, dried over anhydrous sodium sulfate and evaporated to give a brown solid N,N-dimethyl-(R)-1- [(S)-2-(diphenylphosphino)ferrocenyl]ethylamine crude,Recrystallization from ethanol gave a pale yellow solid N,N-dimethyl-(R)-1-[(S)-2-(diphenylphosphino)ferrocenyl]ethylamine, N,N-dimethyl The mass ratio of the crude -(R)-1-[(S)-2-(diphenylphosphino)ferrocenyl]ethylamine to ethanol was 1:5; the yield was 82.4%.

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

Reference£º
Patent; Xi’an Modern Chemical Institute; Yang Cuifeng; Chen Tao; Xu Zegang; Mao Mingzhen; Zhang Xiaoguang; Ning Binke; Su Tianduo; Li Bingbo; Wang Yuemei; Wei Tianqi; Zhang Yuanyuan; (7 pag.)CN108456235; (2018); A;,
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.

LiBH4 (22 mg, 1 mmol) and Me6TREN (0.52 mL, 2 mmol) wereadded to 5 mL of THF. This was heated to reflux for 1 h at whichpoint the heat and stirrer were turned off. Slow cooling of the solutionyielded X-ray quality colorless crystals (40 mg, 16%).1H NMR (400.1 MHz, C6D6, 300 K): delta 2.11 (s, 18H, Me6TREN Me),1.94, 1.90 (overlapping br s, 12H, Me6TREN CH2), 0.59 ppm(quartet/septet, 4H, BH4, 1J10BH = 27.5 Hz, 1J11BH = 81.5 Hz).13C NMR (100.6 MHz, C6D6, 300 K): delta 57.0 (CH2), 51.2 (CH2),45.7 ppm (Me).7Li NMR (155.5 MHz, C6D6, 300 K): delta 0.29 ppm.11B NMR (128.3 MHz, C6D6, 300 K): delta 39.5 ppm (quin,1JBH = 81.2 Hz).Elemental analysis for C12H34N4LiB: Calc.: C, 57.15; H, 13.59; N,22.22. Found: C, 57.16; H, 13.48; N, 22.59%.

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

Reference£º
Article; Kennedy, Alan R.; McLellan, Ross; McNeil, Greg J.; Mulvey, Robert E.; Robertson, Stuart D.; Polyhedron; vol. 103; (2016); p. 94 – 99;,
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

33527-91-2, Tris[2-(dimethylamino)ethyl]amine is a chiral-nitrogen-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: The copper complex Cu5-1 was dissolved in water, and an excessive amount of an aqueous solution of saturated sodium tetrafluoroborate (manufactured by Wako Pure Chemical Industries, Ltd.) was added while stirring. A precipitated solid was collected by filtering and a copper complex Cu5-72 was obtained.

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

Reference£º
Patent; FUJIFILM Corporation; Sasaki, Kouitsu; Kawashima, Takashi; Hitomi, Seiichi; Shiraishi, Yasuharu; US10215898; (2019); 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

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

Add in a 100mL single-mouth bottleN1,N2-dimethylethyl-1,2-diamine (4g, 45mmol), cooled to about 0 C in an ice bath,Then (Boc) 2O (5 g, 23 mmol) in DCM (20 mL)The temperature was raised to 25 C and the reaction was stirred for 4 h.Concentrated under reduced pressure, a saturated sodium carbonate solution was added to the residue, and extracted three times with ethyl acetate (30 mL¡Á3).The organic phase was combined, washed three times with saturated brine (20 mL¡Á3) and dried over anhydrous sodiumThe mixture was suction filtered under reduced pressure, and the filtrate was evaporated.The crude product was purified by column chromatography eluting with EtOAc EtOAcConcentration under reduced pressure gave 2.1 g of a yellow oil.

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

Reference£º
Patent; Beijing Purunao Bio-technology Co., Ltd.; Zhang Peilong; Shi Hepeng; Lan Wenli; Song Zhitao; (250 pag.)CN108707139; (2018); A;,
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