Day: August 27, 2020

10581-12-1, Tetramethylammonium acetate is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: The appropriate ligand (H3LR)(0.18 mmol, R=OMe, Me H, Cl, Br), was deprotonated with 3.1 molar equiv. KH in3mL of DMA in a 25-50-mL round bottom flask. After H2 evolution ceased (?5-10 min), an excess 1.2 eq of Mn(OAc)2 was added along with 1mL of DMA andstirred for 30 min. Then 2.1 equivalents of [Me4N][OAc] were added along with 1mL ofDMA and the reaction was stirred at room temperature overnight. The mixture was filteredthrough a glass fritted funnel to remove insoluble material. The filtrate was layeredunder Et2O and allowed to stand for recrystallization. In most cases a whitecrystalline solid was obtained and isolated by filtration. In some cases, an oily residuewas obtained that through trituration with Et2O and scraping yields a white solid. Ineither case, the solids from DMA/Et2O was then redissolved in acetonitrile and filteredto remove insoluble material. Recrystallization was accomplished by slow vapor diffusionof Et2O into acetonitrile. The solids obtained were washed with diethyl ether anddried under vacuum. See below for characterization data for the remainingMn(II) complexes. [Me4N]2[MnLBr(OAc)]. Yield: 83%. ATR-FTIR (cm-1): 3026, 2890, 2832, 1586, 1552.Anal Calcd for [Me4N]2[MnLBr(OAc)] MnC34H45N6O5Br3: C 44.76; H 4.97; N 9.21. Found:C 44.78; H 4.97; N 9.22. HRMS (LDI/FT-ICR) m/z: Calcd for [MnLBr]- (MnC24H18N4O3Br3)703.84715; Found 703.83080.

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

Reference£º
Article; Cannella, Anthony F.; Surendhran, Roshaan; MacMillan, Samantha N.; Gupta, Rupal; Lacy, David C.; Journal of Coordination Chemistry; vol. 72; 8; (2019); p. 1287 – 1297;,
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.485-71-2,Cinchonidine,as a common compound, the synthetic route is as follows.

Preparation method of this embodiment Example 1 is the preparation method of compound 3a, which specifically includes the following steps: 0.5 mmol of cinconidine(1), 0.6 mmol of acetic acid (2a), 0.6 mmol of DCC, and 0.1 mmol of DMAP In a 50mL flask, then add dichloromethane (10mL) dried with calcium hydride, and then react at room temperature. The reaction process was followed by TLC to detect that the raw material (cinconidine) was complete. The reaction was completed. Urea gives the filtrate. The filtrate was then diluted with 50 mL of dichloromethane to obtain a dilution solution. The dilution solution was washed with 30 mL of 0.1 mol / L hydrochloric acid, 30 mL of a saturated sodium bicarbonate solution, and 30 mL of a saturated saline solution successively, and then dried over anhydrous sodium sulfate. . Then, the solvent (dichloromethane) was removed from the dried diluent under reduced pressure, and then separated by silica gel column chromatography (eluent was a mixed solution of ethyl acetate and petroleum ether with a volume ratio of 1: 1) to obtain compound 3a. The yield is 39%.

485-71-2 Cinchonidine 101744, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Patent; Henan University of Science and Technology; Che Zhiping; Tian Yuee; Chen Genqiang; Liu Shengming; Lin Xiaomin; Jiang Jia; Sun Di; Yang Jinming; (22 pag.)CN110642855; (2020); A;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

4730-54-5, 1,4,7-Triazacyclononane is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

1.0 g (7.8 mmol) of 1,4,7-triazacyclononane and 16.7 mL of mesitylene were supplied into a 50 mL two-necked flask equipped with a reflux condenser, and 4.8 g (27 mmol) of cyclohexylmethyl bromide and 2.2 g (39 mmol) of potassium hydroxide were added. The mixture was stirred for 72 hours at 100 C. under argon gas atmosphere. After reaction completed, salt was removed by filtration, and then the filtrate was concentrated and purified by reduced-pressure distillation. (Amount of yield 2.7 g, Yield 83%) [0092] 1H-NMR(chloroform-d,ppm):0.75-1.90(m,33H), 2.23(d,6H), 2.68(s,12H) [0093] 13C-NMR(chloroform-d,ppm):26.6, 27.3, 32.3, 36.9, 57.0, 67.0 IR(KBr method, cm-1): 2919, 2849, 2788, 1448, 1357, 1314, 1263, 1161, 1113, 1033, 997, 965, 892, 843, 792, 728 [0094] Elemental analysis/calculated value: C(77.63%), H(12.31%), N(10.06%)/observed value: C(78.02%), H(12.43%), N(9.89%) [0095] (ii) Synthesis of Cu(cHexMe3tacn): [0096] To 0.36 g (0.86 mmol) of 1,4,7-tris(cyclohexylmethyl)-1,4,7-triazacyclononane, 10 mL of dichloromethane/methanol was added to obtain a uniform solution, and then 5 mL of dichloromethane/methanol containing 0.15 g (0.88 mmol) of cupric chloride dehydrate was added. The mixture was stirred for one hour at room temperature. After reaction completed, solvent was removed in vacuum, and then the residue was recrystallized from dichloromethane/methanol. (Amount of yield 0.28 g, Yield 59%) [0097] IR(KBr method, cm-1):2929, 2922, 2916, 2849, 1496, 1447, 1106, [0098] Elemental analysis/calculated value: C(58.74%), H(9.31%), N(7.61%)/observed value: C(58.35%), H(9.25%), N(7.58%)

The synthetic route of 4730-54-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Higashimura, Hideyuki; Kotake, Eiichi; Kubota, Masaaki; Kobayashi, Shiro; US2004/267057; (2004); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

4730-54-5, 1,4,7-Triazacyclononane is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture of 6a (30 mg, 0.078 mmol), 1,4,7-triazacyclononane (3.4 mg, 0.026 mmol), K2CO3 (18.1 mg, 0.13 mmol), MeCN (1.2 mL) and CH2Cl2 (0.2 mL) was stirred overnight at r.t. The solvents were evaporated and the product purified by preparative TLC (10 % EtOH/CH2Cl2 + 1 % TEA), yielding 24 mg (89 %) of the title compound.ESI-TOF-MS [M+H]+: calc. for C54H6IN6Oi5+ 1033.42, found 1033.42.

4730-54-5 1,4,7-Triazacyclononane 188318, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Patent; WALLAC OY; WO2009/30819; (2009); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

137076-54-1, 2-(4,7,10-Tris(2-(tert-butoxy)-2-oxoethyl)-1,4,7,10-tetraazacyclododecan-1-yl)acetic acid is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The procedure that was followed was described in Li, C, et al., J. Am. Chem. Soc, 2006, 128, 15072-73. Compound 2-(4,7,10-Tris(2-(tert-butoxy)-2-oxoethyl)-1,4,7,10-tetraazacyclododecan-1-yl)acetic acid (400 mg, 0.70 mmol), N-hydroxysuccinimide (90.4 mg, 0.78 mmol, 1.1 equiv.), and O-benzotriazol-1-yl-N,N,N’,N-tetramethyluronium hexafluorophosphate (HBTU) (296 mg, 0.78 mmol, 1.1 equiv.) were dissolved in 10 mL of acetonitrile. The reaction was stirred at room temperature for 24 hr. After removing the solvent under vaccum, the crude product was purified by flash chromatography on silica gel (CH2Cl2/MeOH, 85:15) to give compound tri-tert-butyl 2,2′,2″-(10-(2-((2,5-dioxopyrrolidin-1-yl)oxy)-2-oxoethyl)-1,4,7,10-tetraazacyclododecane-1,4,7-triyl)triacetate as a white foam (404 mg, 86 %) Rf : 0.3 (CH2Cl2/MeOH, 85:15). 1H NMR (300MHz, CDCl3) delta 3.51 (br, 4H, H8), 3.54 (br, 4H, H13, H1′), 3.32-3.26 (m, 4H, H6), 3.08-2.99 (m, 4H, H5), 2.97-2.86 (m, 8H, H2, H3), 2.85 (s, H4′), 1.46 (s, 18H, H12), 1 .45 (s, 9H, H17). 13C NMR (75MHz, CDCl3) delta 173.4 (C9, C14), 173.1 (C2′), 169.9 (C3′), 82.6 (C16), 82.4 (C11), 55.8 (C8), 55.7 (C13), 54.2 (C1′), 54.1 -51 .5 (C2, C3), 51 .0-48.9 (C5, C6), 27.8 (C17), 27.6 (C12). 25.6 (C4′) MS (CI/NH3) m/z 692 [M + H]+

The synthetic route of 137076-54-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; INSTITUT CURIE; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE; UNIVERSITE PIERRE ET MARIE CURIE (PARIS 6); FLORENT, Jean-Claude; AIT SARKOUH, Rafik; JOHANNES, Ludger; SCHMIDT, Frederic; OBERLEITNER, Birgit; DRANSART, Estelle; SEMETEY, Vincent; WO2014/86942; (2014); 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.4730-54-5,1,4,7-Triazacyclononane,as a common compound, the synthetic route is as follows.

To a solution of acetic acid 2-acetoxy-2-[3-(allyl-methyl-carbamoyl)-5- chlorocarbonyl^Atheta-triiodo-phenylcarbamoyll-ethyl ester (17) (3.7g, 5.10mmol) in dichloromethane (2OmL) was added 1 ,4,7-triazacyclononane (200mg, 1.55mmol) followed by triethylamine (650mul_, 5.10mmol). The reaction mixture was stirred at 5O0C for 48h. After cooling to ambient temperature, ethyl acetate (5OmL) was added, and the white precipitate collected. Purification by column chromatography, eluting with ethyl acetate:methanol(10 – 50%, 12 column volumes, SiO2, 25Og) gave the desired product as an off white solid (2g, 53%). LCMS was carried out Luna C18 250 LCMS shown one major peak with a mass of 1215.83 (M/2 + H+) and a purity of 85%.

4730-54-5 1,4,7-Triazacyclononane 188318, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Patent; GE HEALTHCARE AS; WO2008/123779; (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.7325-46-4,2,2′-(1,4-Phenylene)diacetic acid,as a common compound, the synthetic route is as follows.

Step 1: (0447) The reaction flask was charged with 2,2?-(1,4-phenylene)diacetic acid 30-a (9.2 g, 47.4 mmol) and ethanol (50 ml), concentrated sulfuric acid (5 ml, 94.8 mmol) was slowly added dropwise under stirring. The mixture was stirred at 80 C. overnight and then concentrated under reduced pressure to remove ethanol. Dichloromethane was added and the pH value of the aqueous layer was adjusted to 8 with saturated sodium bicarbonate solution. The aqueous phase was separated and extracted again with dichloromethane. The combined organic phase was dried and concentrated to give 30-b as solid (10.3 g, yield: 87%). ESI-MS (m/z): 251.2 [M+H]+.

As the paragraph descriping shows that 7325-46-4 is playing an increasingly important role.

Reference£º
Patent; SHANGHAI INSTITUTE OF MATERIA MEDICA, CHINESE ACADEMY OF SCIENCES; SUZHOU VIGONVITA LIFE SCIENCES CO., LTD.; TOPHARMAN SHANDONG CO., LTD.; JIANG, Hualiang; WANG, Zhen; LI, Jianfeng; ZHANG, Rongxia; HE, Yang; LIU, Yongjian; BI, Minghao; LIU, Zheng; TIAN, Guanghui; CHEN, Weiming; YANG, Feipu; WU, Chunhui; WANG, Yu; JIANG, Xiangrui; YIN, Jingjing; WANG, Guan; SHEN, Jingshan; (70 pag.)US2017/158680; (2017); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

54761-04-5, Ytterbium(III) trifluoromethanesulfonate is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 2 Preparation of Ru(OTf)[(S,S)-Tsdpen](p-cymene) as Sulfonate Complex First, Ru[(S,S)-Tsdpen](p-cymene) (180 mg, 0.3 mmol), Yb(OTf)3 (183 mg, 0.3 mmol) (manufactured by Aldrich), and 3 ml of CH3OH were charged in a 20 ml Schlenk-type reaction tube purged with argon. Then, the resultant mixture was degassed and stirred at room temperature for 10 minutes. After CH3OH was distilled off under reduced pressure (1 mm Hg), 2 ml of THF was added to the residue, and the produced precipitate was filtered off, washed with 1 ml of THF and with 5 ml of toluene, and dried under reduced pressure (1 mmHg) to obtain 130 mg of Ru(OTf)[(S,S)-Tsdpen](p-cymene).

As the paragraph descriping shows that 54761-04-5 is playing an increasingly important role.

Reference£º
Patent; NAGOYA INDUSTRIAL SCIENCE RESEARCH INSTITUTE; US2008/234525; (2008); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

78902-09-7, 2-(2,2-Diethoxyethyl)isoindoline-1,3-dione is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2-{2,2-bis[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]ethyl}-1H-isoindole-1,3(2H)-dione (Compound 5) To a mixture of phthalimidoacetaldehyde diethyl acetal (3.5 g, 13.3 mmol) and cis,cis-9,12-octadecadien-1-ol (10.6 g, 39.9 mmol) was added pyridinium p-toluenesulfonate (0.167 g, 0.665 mmol) and heated to 105 C. After 48 h, the reaction was diluted in 300 ml of dichloromethane. The organic was washed by 100 ml of saturated sodium bicarbonate solution twice and brine (100 ml). The organic layer was dried over sodium sulfate, filtered and concentrated. The residue was purified by silica gel chromatography (0% ethyl acetate/hexane ?20% ethyl acetate/hexane) to give the title compound (7.6 g). MS 726.6 (M+Na).

78902-09-7 2-(2,2-Diethoxyethyl)isoindoline-1,3-dione 315286, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Patent; SIRNA THERAPEUTICS, INC.; Colletti, Steven L.; Deng, Zhengwu James; Stanton, Matthew G.; Wang, Weimin; Hills, Ivory; (47 pag.)US9670487; (2017); B2;,
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.54761-04-5,Ytterbium(III) trifluoromethanesulfonate,as a common compound, the synthetic route is as follows.

To 5 (0.131 g, 1.0 mmol) and Yb(OTf)3 (0.124 g, 0.20 mmol) in CH2Cl2 (1.5 mL) under argon was added methyl vinyl ketone 22(0.162 mL, 2 mmol). The reaction mixture was stirred at rt overnight and concentrated in vacuo. Purification by silica gel chromatography (1:1, EtOAc:hexane, to 100%, EtOAc, as eluent) afforded 24 asa white solid (0.051 g, 25%) and 23 as a yellow oil (0.128 g, 37%): Rf.0.23 (1:1, EtOAc:methanol, as eluent); 1H NMR (700 MHz, CDCl3)d 9.12 (br s, 1H), 7.87 (dd, J7.6, 1.1 Hz, 1H), 7.72 (td, J7.6, 1.1 Hz,1H), 7.47 (td, J7.6, 1.1 Hz, 1H), 7.35 (dd, J7.6, 1.1 Hz, 1H), 4.32 (t,J6.0 Hz, 2H), 4.14 (t, J8.1 Hz, 2H), 3.29 (t, J6.0 Hz, 2H), 3.27 (t,J8.1 Hz, 2H), 2.23 (s, 3H) ppm; 13C NMR (176 MHz, CDCl3) d 206.2,168.1, 138.6, 136.4, 134.7, 128.7 (q, J285 Hz), 124.7, 121.9, 119.4,116.8, 55.6, 49.2, 40.1, 30.1, 25.5; IR nmax (thin film) 1714 (C]O),1661 (C]N) cm1; LRMS (TOF ES), 203.5 (100%) [MH], 201.7(70%), 132.1 (25%); LRMS (TOF ES-), 149.0 (100%) [OTf]; HRMS(FTMS ES) calculated for C13H15NOH, 202.12264; found202.12262; HRMS (FTMS ES-), calculated for CF3O3Se, 148.95257;found 148.95217.

54761-04-5 Ytterbium(III) trifluoromethanesulfonate 2733225, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Article; Girling, P. Ricardo; Batsanov, Andrei S.; Calow, Adam D.J.; Shen, Hong C.; Whiting, Andrew; Tetrahedron; vol. 72; 8; (2016); p. 1105 – 1113;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI