Month: September 2020

4479-74-7, 2,2-Bipyridine-6,6-dicarboxylic Acid is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A mixture of Tb(NO3)3¡¤6H2O (0.045 g, 0.10 mmol), H2bpdc (0.024 g, 0.10 mmol) in distilled water (10 mL) that adjusted the pH value to 2.5 with 0.5 mol L-1 NaOH aqueous solution. It was then sealed in a 25 mL Teflon reactor and heated at 160 C for 72 h, and then cooled to ambient temperature at a rate of ca.2 C h-1 to give colorless block crystals of 7, yield: 57% based on H2bpdc.

4479-74-7, The synthetic route of 4479-74-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Ren, Ya-Lan; Wang, Fei; Hu, Huai-Ming; Chang, Zhuguo; Yang, Meng-Lin; Xue, Ganglin; Inorganica Chimica Acta; vol. 434; (2015); p. 104 – 112;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.29841-69-8,(1S,2S)-(-)-1,2-Diphenylethylenediamine,as a common compound, the synthetic route is as follows.

trans-RuH(eta1-BH4)[(s)-xylbinap][(S,S)-dpen] was synthesized. First, trans-RuCl2[(S)-xylbinap][(S,S)-dpen] was synthesized. That is, [RuCl2(benzene)]2 (62.5 mg; 0.125 mmol) (made by Aldrich Inc.) and (R)-XylBINAP (183.5 mg; 0.25 mmol) were weighed and placed in a 75 mL Schlenk reaction tube equipped with a stirrer coated with polytetrafluoroethylene, and after depressurizing the interior of the vessel to eliminate air, argon was introduced. After then adding DMF (3 mL) with a syringe, heating in an oil bath set to 100 C. was performed for 10 minutes under an argon atmosphere. After cooling the reaction solution to room temperature, DMF was distilled off under reduced pressure(1 mmHg). (S, S)-DPEN (53.0 mg; 0.25 mmol) (made by Kankyo Kagaku Center Co., Ltd.) and methylene chloride (3 mL) were then added under an argon gas flow to the reddish-brown RuCl2[(S)-xylbinap] (dmf)n solution thus obtained and stirring at 25 C. was performed for 1 hour. A green-colored crude product obtained by distilling off the methylene chloride under reduced pressure (1 mmHg) was dissolved in a 1:1 volume ratio methylene chloride/diethyl ether mixed solvent (2 mL) and this was passed through a column packed with silica gel (5 g) using a 1:1 volume ratio diethyl ether-hexane solution as an eluate to remove impurities. A yellow solution obtained as a precursor was then concentrated until a complex precipitated and solids were separated by filtration and dried under reduced pressure (1 mmHg) to obtain trans-RuCl2[(S)-xylbinap][(S,S)-dpen] (214.8 mg; 0.192 mmol; yield: 77%) as a yellow powder. [XylBINAP] and [xylbinap] are abbreviations for 2,2′-bis(di-3,5-xylylphosphino)-1,1′-binaphthyl. [00032] The abovementioned trans-RuCl2[(S)-xylbinap] [(S,S)-dpen] (89.5 mg; 0.08 mmol) and sodium borohydride (75.6 mg; 2.0 mmol) (made by Nacalai Tesque, Inc.) were then weighed and placed in a 20 mL Schlenk reaction tube equipped with a stirrer coated with polytetrafluoroethylene, and after depressurizing the interior of the vessel to eliminate air, argon was introduced. After then adding a 1:1 volume ratio mixed solvent of benzene/ethanol (6 mL) with a syringe, heating in an oil bath set to 65 C. was performed for 5 minutes under an argon atmosphere. The reaction solution was thereafter stirred for 30 minutes at room temperature. After then drying and solidifying the crude product by distilling off the solvent under reduced pressure (1 mmHg), hexane (5 mL) was added under an argon gas flow to dissolve as much of a yellow product as possible and then the excess sodium borohydride was eliminated by filtration by celite (0.5 g). A yellow filtrate thus obtained was concentrated to approximately 1 ml by depressurization (1 mm Hg) and yellow solids thus precipitated were separated by filtration through a glass filter and dried under reduced pressure (1 mmHg) to obtain trans-RuH(eta1-BH4)[(S)-xylbinap][(S,S)-dpen] (38.3 mg; yield: 45%; see formula (4) below) as a yellow powder. Decomposition temperature: 220 C.; 1HNMR(400 MHz, C6D6) delta-13.67(t, 1, J=23.2 Hz, RuH), -0.48(brs, 4, BH4), 1.59(brs, 12, 4 CH3), 1.78(s, 6, 2CH3), 2.00(s, 6, 2CH3), 2.28-2.35(m, 2, 2NHH), 3.62-3.67(m, 1, CHNH2), 3.76-3.81(m, 2,2CHNH2), 4.09 (dd, 1, J=9.6 and 18.2 Hz, CHNH2), 5.77-8.38(m, 34, aromatics); 31PNMR(161.7 MHz, C6D6) delta73.1(d, J=41.4 Hz), 76.8(d, J=41.4 Hz); IR(toluene)2319(s), 1850(s), 1125(s)cm-1; ESI-MS m/z1063.33([M-H]+), theoretical value (C66H68BN2P2Ru): 1063.40.

29841-69-8, 29841-69-8 (1S,2S)-(-)-1,2-Diphenylethylenediamine 6931238, acatalyst-ligand compound, is more and more widely used in various fields.

Reference£º
Patent; Nagoya Industrial Science Research Institute; US6720439; (2004); B1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

29176-55-4, 2,9-Dichloro-1,10-phenanthroline is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: An oven-dried Schlenk flask was evacuated and back-filled with argon three times. (Hetero)aryl (di)halide (1 equiv), base (1.5 equiv per halogen) and a solution of SPO (1.2 equiv per halogen) in anhydrous solvent (5 mL/mmol per halogen) were added to the flask. The solution was bubbled with argon for 10 min and Pd(OAc)2 (1 mol% per halogen) and ferrocene-based bidentate phosphine ligand (2 mol% per halogen) were added to the flask simultaneously [2.5 mol% Pd(OAc)2 per halogen and 5 mol% dppf per halogen for compounds 2j, 2l, 2r, 2t, 2w]. The resulting mixture was heated at the indicated temperature for the given time. Workup procedures are described below for two different conditions. Final purification of crude products was achieved by column chromatography on silica gel (40-60 mum) using CH2Cl2-MeOH as eluent. Reaction scale and yields are shown in Table 1 (2a-w), Scheme 1 (3a-h) and Scheme 2 (4a-g). Notice that all compounds with two phosphine oxide groups are beige-to-brown solids or slowly solidifying viscous brown oils. Conditions I: ligand: dppf, solvent: DMF, base: Cs2CO3 (2d-n, 2q, 2r, 2t-w, 4a-g) or K2CO3 (3a-h), temperature: 120 C, time: 7 h (20 h for 2j, 2l, 2r, 2w). Workup: after cooling, the reaction mixture was poured into a fourfold excess of brine. The mixture was extracted three times with CH2Cl2 (40 mL/mmol each). The combined organic layers were washed with brine to remove traces of DMF, dried over Na2SO4 and then evaporated to dryness. Conditions II: ligand: dippf, solvent: toluene, base: t-BuOK, temperature: 110 C, time: 7 h. Workup: after cooling, the reaction mixture was evaporated to dryness. Then, the mixture was diluted with CH2Cl2 (40 mL/mmol) and washed with water and brine (40 mL/mmol). The organic layer was dried over Na2SO4 and the CH2Cl2 was removed under reduced pressure.

29176-55-4, As the paragraph descriping shows that 29176-55-4 is playing an increasingly important role.

Reference£º
Article; Zakirova, Gladis G.; Mladentsev, Dmitrii Yu.; Borisova, Nataliya E.; Synthesis; vol. 51; 11; (2019); p. 2379 – 2386;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.10581-12-1,Tetramethylammonium acetate,as a common compound, the synthetic route is as follows.

To a solution of compound 3 (20g, 42.8mmol, 1.0eq) in Toluene (200mL) was added tetra methyl ammonium acetate (14.3g, 54.8mmol, 1.28eq) at rt. The mixture was heated to reflux for 16h. TLC analysis indicated formation of a polar spot. Then the reaction mass was extracted with EtOAc (2 X 200m L) and washed with water (2 X 100ml_) and brine (2 X 100ml_). The organic layer was dried under reduced pressure. The residue (40 g) was taken up with 80ml_ of 2-prpoanol. The mixture was stirred at 0C for 30 mins and the resulting Crystalline product was collected under dried under vaccum to give compound 4 (12 g, 68%) as a pale yellow color Solid. LCMS: 79.34% with m/z 356.24 (M+H):

10581-12-1, As the paragraph descriping shows that 10581-12-1 is playing an increasingly important role.

Reference£º
Patent; ONTARIO INSTITUTE FOR CANCER RESEARCH (OICR); AL-AWAR, Rima; ISAAC, Methvin; CHAU, Anh My; MAMAI, Ahmed; WATSON, Iain; PODA, Gennady; SUBRAMANIAN, Pandiaraju; WILSON, Brian; UEHLING, David; PRAKESCH, Michael; JOSEPH, Babu; MORIN, Justin-Alexander; (441 pag.)WO2019/153080; (2019); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.115754-62-6,((1,3-Dioxolan-2-yl)methyl)tributylphosphonium bromide,as a common compound, the synthetic route is as follows.

5.0 g (0.02548 mol) of 3,4,5-trimethoxy benzaldehyde and 33 ml of a 1M solution of previously made Wittig Salt III [4] in dimethylformamide (DMF) (1.3 equivalents, 0.03312 mol) was added to 150 ml 95% EtOH under N2 and warmed to dissolve all solids. 19 ml 2M NaOEt (1.5 equivalents, 0.03822 mol) was added drop-wise, and the reaction was heated to 60 C. for 48 hours. The mixture was poured into 300 ml H2O, extracted with 3¡Á75 ml EtOAc, washed with 2¡Á40 ml H2O and 2¡Á40 ml brine, dried with MgSO4, and concentrated by rotary evaporation. The resulting yellow solids were added to 150 ml THF. 100 ml 2M HCl was added to this solution and stirred for one hour at 20 C. Most of the solvent was removed by rotary evaporation, and the remainder was poured into 100 ml H2O. The product was extracted, washed, and dried as before, giving 5.2 g of impure yellow oil. This oil was purified through a short silica gel column, eluting with CH2Cl2 giving 4.02 g of a yellow solid, (E)-4-(3,4,5-trimethoxyphenyl)but-3-en-2-one intermediate product. The total yield was 4.02 g or 71%.1H NMR (500 MHz, CDCl3), delta 9.66 (d, J=8 Hz, 1H), 7.37 (d, J=16 Hz, 1H), 6.77 (s, 2H), 6.62 (dd, J=16 Hz, J=8 Hz, 1H), 3.88 (s, 9H), 115754-62-6

115754-62-6 ((1,3-Dioxolan-2-yl)methyl)tributylphosphonium bromide 22292430, acatalyst-ligand compound, is more and more widely used in various fields.

Reference£º
Patent; Spangler, Brenda D.; Spangler, Charles W.; Tarter, E. Scott; US2009/43109; (2009); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.10581-12-1,Tetramethylammonium acetate,as a common compound, the synthetic route is as follows.

General procedure: A solution of H3F3ST (300mg, 0.39mmol) dissolved in 6mL of anhydrous dimethylacetamide (DMA) was treated with solid NaH (28mg, 1.2mmol). The mixture was stirred until gas evolution ceased. Fe(OAc)2 (68mg, 0.39mmol) and NMe4OAc (52mg, 0.39mmol), were added to the cloudy white reaction, and the solution was stirred. After 3h, 5mL of Et2O was added to the yellow solution to aid the precipitation of NaOAc. The reaction mixture was filtered through a medium porosity glass-fritted funnel to remove the insoluble species and the filtrate was dried under vacuum. The resulting pale yellow solid was redissolved in 5mL of acetonitrile (MeCN), stirred for 20min, and filtered using a fine porosity glass-fritted funnel. The filtrate was concentrated under vacuum to ca. 1mL and treated with Et2O (10mL) then pentane (40mL) to precipitate a pale yellow solid. The pale yellow solid was collected on a medium porosity glass-fritted funnel and dried under vacuum to give 182mg (91%) of product., 10581-12-1

10581-12-1 Tetramethylammonium acetate 82741, acatalyst-ligand compound, is more and more widely used in various fields.

Reference£º
Article; Lau, Nathanael; Ziller, Joseph W.; Borovik; Polyhedron; vol. 85; (2015); p. 777 – 782;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.23616-79-7,N-Benzyl-N,N-dibutylbutan-1-aminium chloride,as a common compound, the synthetic route is as follows.

EXAMPLE 3 A 3-necked, 250 mL round-bottomed flask equipped with a reflux condenser and two pressure equalizing addition funnels was charged with 60 mL of a 30 percent by weight aqueous sodium hydroxide solution and 1.275 gram (4.1 mmol) of benzyltributylammonium chloride. 4-hydroxymethyl-2-methoxy-2-methyl-1,3-dioxolane (29.14 g, 196.7 mmol) and 25 g vinylbenzyl chloride (164 mmol) were simultaneously charged under a nitrogen atmosphere from the addition funnels into the flask over a 5 minute period. The reaction flask was immersed in an oil bath at 50 C. and the contents were stirred for 6 hours, then stirred at room temperature overnight. The organic phase was separated, diluted with methylene chloride (200 mL) and triethylamine (5 mL), washed with water, dried over anhydrous magnesium sulfate, and vacuum stripped. 42 g of 4-hydroxymethyl-2-methoxy-2-methyl-1,3-dioxolane vinylbenzyl ether were produced.

23616-79-7, 23616-79-7 N-Benzyl-N,N-dibutylbutan-1-aminium chloride 159952, acatalyst-ligand compound, is more and more widely used in various fields.

Reference£º
Patent; General Electric Company; US5231197; (1993); A;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

1662-01-7, 4,7-Diphenyl-1,10-phenanthroline is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Synthesis of 2,4,7-triphenyl-1,10-phenanthrolineTo a three-necked flask of 250 ml, 0.97 g (6.16 mmol) of bromobenzene and 70 ml of THF were charged, then 3.9 ml (22 mmol) n-butyllithium (1.6M in Hexane solution) was dropped under stirring at -78 C. in a nitrogen atmosphere. The mixture was stirred for one hour at -78 C., and a solution of 1.86 g (5.6 mmol) 4,7-diphenyl-1,10-phenanthroline in 30 ml THF was dropped. Then the mixture was stirred at room temperature for overnight and was added with water. The organic layer was extracted with Dichloromethane and dried with anhydrous magnesium sulfate, the solvent was removed by rotary evaporation. The product was purified by column chromatography on alumina using Dichloromethane/Hexane as eluent and dried in vacuo, obtaining white powder compound 0.85 g (yield of 37.21%).

1662-01-7, 1662-01-7 4,7-Diphenyl-1,10-phenanthroline 72812, acatalyst-ligand compound, is more and more widely used in various fields.

Reference£º
Patent; Yen, Feng Wen; US2008/265746; (2008); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.168646-54-6,5,6-Diamino-1,10-phenanthroline,as a common compound, the synthetic route is as follows.

5mmol of Phen-NH2, 5.5mmol of indoline-2,3-dione and 0.1mmol of 4-methylbenzenesulfonic acid were added into 25mL of ethanol and heated to reflux overnight. After cooling, the solution was poured into 300mL of cold water. The crude product was collected and recrystalized in ethanol to yield IPP as gray powder. 1H NMR (300Hz, CDCl3, 25¡ãC): delta 10.13 (d, 1H, J=8.5Hz), 9.24 (d,1H, J=2.5Hz), 9.17 (d, 1H, J=2.0Hz), 9.09 (d, 1H, J=5.5Hz), 8.55 (d, 1H, J=5.5Hz), 7.60?7.64 (m, 2H), 7.55 (d, 1H, J=8.5Hz), 7.34 (m, 2H). Anal. Calcd for C20H11N5: C, 74.76; H, 3.45; N, 21.79. Found: C, 74.67, H, 3.60; N, 21.68., 168646-54-6

As the paragraph descriping shows that 168646-54-6 is playing an increasingly important role.

Reference£º
Article; Li, Xiaogang; Zhang, Dong; Li, Jing; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 127; (2014); p. 1 – 9;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.29841-69-8,(1S,2S)-(-)-1,2-Diphenylethylenediamine,as a common compound, the synthetic route is as follows.

Example 4: Preparation of RuCI [ (1 S, 2S)-p-dansylNCH (C6H5) CH (C6H5) NH2] (rl6-p-cymene) a) Preparation of (S, S)-5-dimethylamino-naphthalene-1-sulfonic acid (2-amino-1, 2-diphenyl- ethyl)-amide : To a solution of (S, S)-diphenylethylenediamine (250 mg, 1.2 mmol) and triethylamine (0.5 ml) in THF is added dropwise a solution of dansyl chloride (318 mg, 1.2 mmol) in THF (2 mi) at 0C. After stirring 16 h at RT the solvent is removed in vacuum and the residue is resolved in methylenchloride (20 ml). The organic solution is washed with NaHCO3 solution (5 ml), dried over Na2SO4 and after filtration the solvent is removed. Flash chromatographie afford (S, S)-5-dimethylamino-naphthalene-1-sulfonic acid (2-amino-1,2- diphenyl-ethyl)-amide as yellow oil which crystallizes by drying in vacuum. M: 445. 59. in- NMR (400 MHz, CDCl3) : 8.36 (t, J = 7.5 Hz, 2 H), 8.17 (dd, J = 7.2, 1.2 Hz, 1 H), 7.47 (dd, J = 8.8 Hz, 1 H), 7. 34 (dd, J = 8.5 Hz, 1 H), 7.24-7. 16 (m, 4 H), 7.11 (d, J = 7.5 Hz, 1 H), 6.99- 6.74 (m, 6 H), 4.61 (d, J = 8.5 Hz, 1 H), 4.20 (d, J = 8.5 Hz, 1 H), 2.80 (s, 6 H)

29841-69-8, The synthetic route of 29841-69-8 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2005/92294; (2005); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI