Day: September 29, 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1121-22-8,trans-Cyclohexane-1,2-diamine,as a common compound, the synthetic route is as follows.

[0444] This ligand has been described by Van Stein, G C; Van Loten, G; Vrieze, K, Inorg. Chem 1985, 24 (9), 1367-1375. [0445] 19.36 g of anhydrous magnesium sulphate (161.1 mmoles) and 6.44 ml of rac-trans-1,2-diaminocyclohexane (53.6 mmoles) were successively added to a solution of 10 ml of 2-thienylaldehyde (107.1 mmoles) in 75 ml of absolute ethanol. [0446] The reaction mixture was stirred for 16 hours at ambient temperature (the solution thickened very rapidly), heated for 2 hours under reflux then filtered through a frit. [0447] The isolated solid was washed with dichloromethane. [0448] The total filtrate was concentrated completely under reduced pressure to isolate a brown solid which was re-crystallised from ethanol. [0449] 14.0 g of beige crystals were obtained, corresponding to a yield of 86%. [0450] The characteristics were as follows: [0451] M.Pt: 173-175 C. (EtOH); [0452] 1H NMR/CDCl3: delta 8.27 (s, 2H, H7,14), 7.27 (m, 2H, H, 2), 7.14 (m, 2H, H5,16), 6.96 (m, 2H, H3,4), 3.32 (m, 2H, H8,13), 1.82 (m, 6H, H10,11 and H carried by carbons 9 and 12 located in the position cis (or trans) with respect to the adjacent nitrogen atoms), 1.44 (m, 2H, H carried by carbons 9 and 12 located in the trans (or cis) position with respect to the adjacent nitrogen atoms). [0453] 13C NMR/CDCl3: delta 154.32 (C7 and C14), 142.54 (C6 to C15), 130.09 (C1 and C2), 128.20 (C5 and C16), 127.18 (C3 and C4), 73.38 (C8 and C13), 32.83 (C9 and C12), 24.44 (C10 and C11).

1121-22-8, 1121-22-8 trans-Cyclohexane-1,2-diamine 43806, achiral-catalyst compound, is more and more widely used in various fields.

Reference£º
Patent; Cellier, Pascal Philippe; Cristau, Henri-Jean; Spindler, Jean-Francis; Taillefer, Marc; US2003/236413; (2003); A1;,
Chiral Catalysts
Chiral catalysts – SlideShare

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.673-06-3,D-Phenylalanine,as a common compound, the synthetic route is as follows.

673-06-3, EXAMPLE 1 (R)-2-Bromo-3-phenylpropanoic Acid Sodium nitrite (27 g in water) is added at 0 C. to a solution of D-phenylalanine (40 g) in a mixture of 48% hydrobromic acid/water (1:1 by volume). The mixture is stirred for 30 minutes at 0 C. and then for 2 hours 30 minutes at a temperature close to 0 C. The reaction mixture is extracted with ether. The organic extracts are washed with water and a saturated sodium chloride solution and then dried over sodium sulphate. After filtration and concentration to dryness, the obtained residue is purified by distillation. (R)-2-Bromo-3-phenylpropanoic acid (33 g) is obtained which has the following characteristics: B.p.1kPa =154 C.; Rf =0.47 (methylene chloride/methanol). The yield is 60%.

As the paragraph descriping shows that 673-06-3 is playing an increasingly important role.

Reference£º
Patent; Institut National de la Sante et de la Recherche Medicale (INSERM); US5591891; (1997); A;,
Chiral Catalysts
Chiral catalysts – SlideShare

A common heterocyclic compound, the chiral-catalyst compound, name is trans-Cyclohexane-1,2-diamine,cas is 1121-22-8, mainly used in chemical industry, its synthesis route is as follows.,1121-22-8

Into a solution containing 1,6-diisocyanatohexane (2.35 grams, 13.95 mmol; obtained from Sigma-Aldrich Fine Chemicals) and anhydrous hexane (100 mL, obtained from Sigma-Aldrich Fine Chemicals) stirring at room temperature was added diethylene glycol butyl ether (2.27 grams, 14.0 mmol, obtained from Sigma-Aldrich Fine Chemicals), which was previously dried over calcium chloride granules, and dibutyltin dilaurate as catalyst (0.095 grams, 0.15 mmol, obtained from Sigma-Aldrich Fine Chemicals). The mixture was stirred and heated to an internal temperature of about 45 C. The progress of the reaction was monitored by 1H-NMR spectroscopy for the consumption of the diethylene glycol butyl ether starting material. The mixture was cooled to about 15 C. internal temperature; thereafter, to this mixture was added dropwise a solution of trans-1,2-diaminocyclohexane (0.80 grams, 7.0 mmol; obtained as a racemic mixture of (1R,2R and (1S,2S) stereoisomers from Sigma-Aldrich Fine Chemicals) dissolved in anhydrous hexane (20 mL). The mixture was stirred for about 30 minutes while warming up to room temperature, and FTIR spectroscopic analysis of a reaction sample indicated no unreacted isocyanate (peak at 2180 cm-1, sample prepared as a KBr pellet). The crystalline product was isolated by vacuum filtration on filter paper, rinsed with hexane, and then dried in air to give 4.82 grams of a white powder (88.8% yield). The product was believed to be of the formulae 1H-NMR spectroscopic analysis of the solid was performed in DMSO-d6 (300 MHz) at 80 C. and indicated the above structure with the following assigned peaks: 0.90 ppm (multiplet, 3 H integration, -OCH2CH2OCH2CH2OCH2CH2CH2CH3); 1.05-1.95 ppm (broad multiplets, 16 H integration, 4 methylene protons from butyl ether terminus, 8 methylene protons from the 1,6-diisocyanatohexane portion, and 4 methylene protons from the cyclohexane ring portion); 3.0 ppm (narrow multiplet, 5 H integration, -NH(CO)NHCH2(CH2)4CH2NH(CO)O and also tertiary methine proton adjacent to urea group on cyclohexane ring); 3.40-3.70 ppm (multiplets, 8 H integration, NH(CO)OCH2CH2OCH2CH2OCH2CH2CH2CH3); 4.10 ppm (singlet, 2 H integration, NH(CO)OCH2CH2OCH2CH2OCH2CH2CH2CH3); 5.60 ppm and 5.70 ppm (each a broad singlet, 1 H integration, urea NH protons); 6.75 ppm (broad singlet, 1 H integration, urethane NH proton). Elemental analysis calculated for C: 58.83%, H: 9.54%, N: 10.83%; found for C: 58.81%, H: 9.58%, N: 12.17%.

As the rapid development of chemical substances, we look forward to future research findings about 1121-22-8

Reference£º
Patent; Xerox Corporation; US2006/122415; (2006); A1;,
Chiral Catalysts
Chiral catalysts – SlideShare

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1121-22-8,trans-Cyclohexane-1,2-diamine,as a common compound, the synthetic route is as follows.

Reference Example 35 Production of (2RS,4aSR,8aSR)-2-ethyldecahydroquinoxaline Relative confi uration Dichloro(pentamethylcyclopentadienyl)iridium (III) dimer (70 mg, 0.090 mmol) and sodium bicarbonate (73 mg, 0.87 mmol) were added to an aqueous (20 mL) solution of trans-cyclohexane-l,2-diamine (2.00 g, 17.5 mmol) and (¡À)-l,2-butanediol (1.69 mL, 18.4 mmol) with stirring at room temperature. Degassing and argon substitution were repeated 3 times, and the mixture was then stirred for 24 hours under reflux. The reaction mixture was concentrated under reduced pressure. The obtained residue was purified by basic silica gel column chromatography (methylene chloride/methanol) to obtain (2R*,4aS*,8aS*)-2- ethyldecahydroquinoxaline (2.03 g, yield: 69%) in a yellow solid form. 1H-NMR(CDCl3)5ppm : 0.92 (3H, t, J = 7.5 Hz), 1.10-1.60 (7H, m), 1.64-1.83 (5H, m), 2.16- 2.31 (2H, m), 2.44 (IH, dd, J = 11.5, 10.4 Hz), 2.58-2.67 (1H, m), 3.02 (1H, dd, J = 11.5, 2.7 Hz)., 1121-22-8

The synthetic route of 1121-22-8 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; OTSUKA PHARMACEUTICAL CO., LTD.; SHINOHARA, Tomoichi; SASAKI, Hirofumi; TAI, Kuninori; ITO, Nobuaki; WO2013/137479; (2013); A1;,
Chiral Catalysts
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602-09-5, [1,1′-Binaphthalene]-2,2′-diol is a chiral-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

NaH (1.92 g, 80 mmol) was added to DMF (30 mL) in an ice bath. BINOL (1,1?-bi-2-naphthol) (10 g , 34 mmol) in THF (50 ml) was dropped to this solution for 20 min. After 30 min, chloromethyl methyl ether (6.4 g, 80 mmol) was dropped to this solution for 20 min. The reaction was monitored by TLC. After 1 h stirring, 3 was isolated from the organic layer by extraction of the reaction mixture with chloroform and water. The product 3 was further purified by silica gel column chromatography with a petroleum ether/ethyl acetate (5/1)mixture. Yield: 90%.1H NMR (400 MHz, CDCl3) delta 7.95-7.93 (d, J = 9.6Hz, 2H), 7.87-7.85 (d, J = 8.4 Hz, 2H), 7.58-7.56 (d, J = 9.6 Hz, 2H),7.35-7.31 (m, 2H), 7.23-7.14 (m, 4H), 5.08-4.96 (q, J = 6.8 Hz, 4H), 3.13 (s,6H)., 602-09-5

602-09-5 [1,1′-Binaphthalene]-2,2′-diol 762831, achiral-catalyst compound, is more and more widely used in various fields.

Reference£º
Article; Zhang, Kewei; Wu, Shengying; Qu, Dahui; Wang, Limin; Tetrahedron Letters; vol. 57; 10; (2016); p. 1133 – 1137;,
Chiral Catalysts
Chiral catalysts – SlideShare

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.602-09-5,[1,1′-Binaphthalene]-2,2′-diol,as a common compound, the synthetic route is as follows.

General procedure: Separately, each of the dihydroxy-substituents, catechol (a), 2,3-dihyroxynaphthalene (b), 2,2′-dihydroxy-1,1′-bisnaphthalene (c) (50 mmol), and NaOH (0.12 mol) were dissolved in 20-25 ml ethanol and 2-chloroethanol (0.12 mol) was added to this solution dropwise over 15 min. After refluxing the reaction mixture for 20 h, the resulting solid was separated by filtration. Ethanol was evaporated in vacuo and the resulting oily product was dissolved in 200 ml chloroform. The chloroform solution was washed with 3% NaOH and then with distilled water until the pH reached neutrality., 602-09-5

The synthetic route of 602-09-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Kertmen, Ahmet; Szczygelska-Tao, Jolanta; Chojnacki, Jaros?aw; Tetrahedron; vol. 69; 49; (2013); p. 10662 – 10668;,
Chiral Catalysts
Chiral catalysts – SlideShare

173035-10-4, 1,3-Dimesityl-4,5-dihydro-1H-imidazol-3-ium chloride is a chiral-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Synthesis of [(SIMes)CuBr]. In an oven-dried vial, copper(I) bromide (0.522 g, 3.63 mmol), SIMes.HCl (0.86 g, 2.52 mmol) and sodium tert-butoxide (0.243 g, 2.52 mmol) were loaded inside a glovebox and stirred in dry THF (18 mL) overnight at room temperature outside of the glovebox. After filtration of the reaction mixture through a plug of Celite, the filtrate was mixed with hexane to form a precipitate. A second filtration afforded 0.808 g (71% yield) of the title complex as an off-white solid.Spectroscopic and analytical data for [(SIMes)CuBr]: 1H NMR (300 MHz, [D6]acetone): delta=7.01 (s, 4H, HAr), 4.16 (s, 4H, NCH2), 2.37 (s, 12H, ArCH3), 2.29 (s, 6H, ArCH3); 13C NMR (75 MHz, CDCl3): delta=202.6 (C, NCN), 138.5 (C, CAr), 135.3 (CH, CAr), 135.0 (C, CAr), 129.7 (CH, CAr), 51.0 (CH2, NCH2), 21.0 (CH3, ArCH3), 18.0 (CH3, ArCH3); Elemental analysis calcd for C21H26BrCuN2 (449.89): C, 56.06; H, 5.83; N, 6.23. Found: C, 55.98; H, 5.64; N, 6.21%., 173035-10-4

The synthetic route of 173035-10-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Institut Catala d’Investigacio Quimica; Institucio Catalana de Recerca i Estudis Avancats; US2009/69569; (2009); A1;,
Chiral Catalysts
Chiral catalysts – SlideShare

602-09-5, [1,1′-Binaphthalene]-2,2′-diol is a chiral-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

602-09-5, Example 26; 1.0 g NaOH, 20 ml water and 2.8 g 2,2′-dihydroxy-1,1′-binaphthyl prepared in the step a) of the Example 19 are added to a round bottom flask with the volume of 100 mL and are then stirred to be dissolved, 4.1 g n-butyl bromine, 0.2 g tetrabutylammonium bromide and 10 ml ethanol are dropwise added to the round bottom flask, the temperature of the water bath is maintained at 70 C., and after the reaction is performed for 4 hours, the reaction product is poured, while hot, into 50 g crushed ice, followed by stirring to further separate crystal out. The crystal is filtered the filter cake is washed with alkali solution and icy water to obtain light yellow granular solid. The solid is recrystallized with ethanol to obtain yellow-white crystal 2,2′-dibutoxy-1,1′-binaphthyl with the yield of 92.3%, the melting point of 85 C. and the content, according to HLPC detection, of 96.6%.

602-09-5 [1,1′-Binaphthalene]-2,2′-diol 762831, achiral-catalyst compound, is more and more widely used in various fields.

Reference£º
Patent; Wang, Licai; Gao, Zhanxian; Li, Wei; Zheng, Guotong; Dong, Qingxin; Liu, Riping; Wang, Xiaohuan; Zhang, Nan; Wang, Jingzhuang; Cai, Shimian; US2011/301385; (2011); A1;,
Chiral Catalysts
Chiral catalysts – SlideShare

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.602-09-5,[1,1′-Binaphthalene]-2,2′-diol,as a common compound, the synthetic route is as follows.

In a glass reactor equipped with a stirrer, cooler and thermometer,286 g (1 mol) of (RS) -1,1′-bi-2-naphthol;194 g (2.2 mol) of ethylene carbonate,Charge 15 g of potassium carbonate and 450 g of toluene,The reaction was performed at 110 C. for 10 hours. After 540 g of toluene was added to this reaction solution to dilute it, 290 g of a 10% by mass aqueous sodium hydroxide solution was added to wash the organic solvent layer. continue,Washing with 500 g of water was repeated until the washed water became neutral. After washing with water, 1.0 g of an aqueous solution of sodium silicate (trade name: sodium silicate solution, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) was added to the organic solvent layer, and the mixture was stirred for 30 minutes. Thereafter, the mixture was cooled from 80 C. to 30 C. at a rate of 0.5 C./min, filtered under reduced pressure (50 kPa) and dried,(RS) -2,2′-bis (2-hydroxyethoxy)-1,1′-binaphthaleneCompound313 g of white crystals(Yield: 83.5% by mass, purity: 99.6%, D50: 55 mum).The silicon content in the obtained crystals was 73 mass ppm., 602-09-5

The synthetic route of 602-09-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; DK Co Ltd; Saito, Daisuke; Umeda, Kazutoshi; (9 pag.)JP6615398; (2019); B1;,
Chiral Catalysts
Chiral catalysts – SlideShare

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.173035-10-4,1,3-Dimesityl-4,5-dihydro-1H-imidazol-3-ium chloride,as a common compound, the synthetic route is as follows.

Synthesis of [(SIMes)CuCl]. This synthesis is as reported in the literature; see S. Diez-Gonzalez et al., J. Org. Chem. 2005, 70, 4784-4796. In a 250 mL Schlenk flask were added copper(I) chloride (1.0 g, 10.10 mmol), 1,3-bis(2,4,6-trimethylphenyl)-4,5-dihydro-imidazol-2-ylidenium chloride (SIMes-HCl, 10.10 mmol), and sodium tert-butoxide (0.97 g, 10.10 mmol). To this flask, dry tetrahydrofuran (100 mL) was added under an inert atmosphere of argon, and the mixture was magnetically stirred for 20 hours at room temperature. After the mixture was filtered through a plug of Celite and then evaporating the solvent under vacuum, a white solid was obtained. 1H NMR (400 MHz, CDCl3) delta=6.96 (s, 4H), 3.96 (s, 4H), 2.32 (s, 12H), 2.30 (s, 6H); 13C NMR (100 MHz, CDCl3) delta=202.8, 138.7, 135.3, 135.0, 129.7, 50.9, 21.0, 18.0. Elemental analysis calcd for C21H26CuClN2: C, 62.21; H, 6.46; N, 6.91. Found: C, 62.60; H, 6.52; N, 6.80%., 173035-10-4

As the paragraph descriping shows that 173035-10-4 is playing an increasingly important role.

Reference£º
Patent; Institut Catala d’Investigacio Quimica; Institucio Catalana de Recerca i Estudis Avancats; US2009/69569; (2009); A1;,
Chiral Catalysts
Chiral catalysts – SlideShare