Tag: M.W:100-200

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1608-26-0,N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine,as a common compound, the synthetic route is as follows.

General procedure: A mixture of 0.8 g of the substrate 1a (4.8 mmol) and 9a(5.2 mmol) in 20 cm3 THF was heated at the reflux temperature for 6 h (TLC), and the excess of the volatile materials was removed under vacuum. The precipitate was collected and washed several times with CH2Cl2 to give the1:1 dipolar adduct 10a. Compound 10a (1.33 g, 85% yield) was pure enough for carrying out the spectroscopic analyses and stable for few days at -10 C. When 10a was quenched with acetic acid containing a catalytic amount of polyphosphoric acid (PPA), and the reaction mixture was heated at 110 C for 2 h (TLC), 2-oxothiazaphosphinane-2-methylamidate (11a) was obtained (0.81 g, 64% yield). 2-Oxothiazaphosphinane-2-ethylamidate (11b) was also obtained (0.91 g, 67% yield) when 1a was allowed to reactwith 9b, using the same conditions and stoichiometric quantities, and was used directly for the second step without separation or identification. 4-Oxo-1(2-[tris(dimethylamino)phosphonio]propyl)-1,4-dihydropyrimidine-2-thiolate (10a, C13H26N5OPS)Yellow substance; m.p.: 177 C (EtOH); 1H NMR(500 MHz, CDCl3): d = 2.83 (d, 3JPH = 9.8 Hz, 18H,[(Me)2N]3P), 1.18 (ddt (m), 3H, MeCP), 4.52-4.60 (m, 2H,H2CN), 5.88, 6.94 (2d, JHH = 7.4 Hz, 2 9 1H, HC5,HC6), 7.32-7.38 (m, 1H, HCP) ppm; 13C NMR (125 MHz,CDCl3): d = 169.9 (C=O), 160.8 (C=N), 135.4 (d,4JPC = 3.8 Hz, C6), 94.9 (C5), 51.4 (d, 2JPC = 12.8 Hz,MeCP), 36.9 (d, 2JPC = 13.7 Hz, [(Me2)N]3P), 22.6 (d,1JPC = 133.2 Hz, CP), 13.6 (d, 2JPC = 11.6 Hz, MeCP)ppm; 31P NMR (200.7 MHz, DMSO-d6): d = 45.7 ppm;IR (KBr): v = 1685 (C=O), 1480 (S-enolic), 1322, 862(PNMe) cm-1; MS (70 eV): m/z (%) = 331 (M+, 54)., 1608-26-0

The synthetic route of 1608-26-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Abdou, Wafaa M.; Kamel, Azza A.; Shaddy, Abeer A.; Monatshefte fur Chemie; vol. 148; 12; (2017); p. 2195 – 2210;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

1608-26-0, N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: To a well-stirred solution of compounds (2a-2b) (2mmol) in anhydrous toluene (15 mL) was added hexamethylphosphoroustriamide (2mmol). The mixture was heated under reflux for 12 h. Silica gel TLC indicated the completion of the reaction. The solvent was evaporated under reduced pressure, and the residue was purified on silica gel preparative TLC using ethyl acetate as eluent. A mixture of compounds (3a-3b) (1mmol), S8 (5 mmol) and anhydrous toluene (10mL) was refluxed for 4h, and then cooled. The sulfur excess was filtered off, and the solvent was removed under reduced pressure. Flash column chromatography on silica gelusing petroleum ether as eluant affords (4a-4b)., 1608-26-0

As the paragraph descriping shows that 1608-26-0 is playing an increasingly important role.

Reference£º
Article; Balti, Monaem; Efrit, Mohamed Lotfi; Journal of Sulfur Chemistry; vol. 37; 4; (2016); p. 466 – 475;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1608-26-0,N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine,as a common compound, the synthetic route is as follows.

General procedure: A mixture of the aminobenzamidine 1 (5.0 mmol) andtris (dimthylamino) phosphine (5.0 mmol) dissolved in anhydroustoluene (10 mL) were heated under reflux for 48 h.After evaporating the solvent in vacuum, the resulting solidproduct was recrystallized from CCl4 (2b, 2d) or alternativelythe obtained oil (2a, 2c) was purified by columnchromatography using silica gel (60-120 mesh) with ethylacetate: petroleum ether (4 : 6) as eluant.

1608-26-0, 1608-26-0 N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine 15355, achiral-phosphine-ligands compound, is more and more widely used in various fields.

Reference£º
Article; Hichri, Sarra; Abderrahim, Raoudha; Letters in Organic Chemistry; vol. 13; 4; (2016); p. 289 – 292;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

1608-26-0, N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A mixture of the aminobenzamidine 1 (5.0 mmol) and tris (dimthylamino) phosphine (5.0 mmol) dissolved in anhydrous toluene (10 mL) were heated under reflux for 48 h. After evaporating the solvent in vacuum, the resulting solid product was recrystallized from CCl4 (2b, 2d) or alternatively the obtained oil (2a, 2c) was purified by column chromatography using silica gel (60-120 mesh) with ethyl acetate: petroleum ether (4 : 6) as eluant., 1608-26-0

As the paragraph descriping shows that 1608-26-0 is playing an increasingly important role.

Reference£º
Article; Hichri, Sarra; Abderrahim, Raoudha; Letters in Organic Chemistry; vol. 13; 4; (2016); p. 289 – 292;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

1608-26-0, N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

In an eggplant-shaped two-neck flask equipped with a reflux condenser, a dropping funnel and a magnetic stirrer, 37.4 g (178 mmol) of diethylsulfate were added dropwise to 24.2 g (149 mmol) of hexamethylphosphorous triamide at room temperature in a nitrogen gas atmosphere. After 3-day stirring at room temperature, a white solid salt was obtained. The salt was washed sufficiently with ether and vacuum-dried at 50 C. for 5 hours to obtain tri(dimethylamino)butylphosphonium butylsulfate with 94% yield.The resulting compound was identified with a nuclear magnetic resonance spectrometer (BRUKER Ultra Shield 300 NMR Spectrometer, supplied by BRUKER Corp.). The spectrum data are shown below.1H-NMR (300 MHz, solvent: acetone-d6, reference material: tetramethylsilane) delta 3.83 (t, 2H) 2.85 (d, 18H) 2.73-2.63 (m, 2H) 1.70-1.33 (m, 8H) 0.97 (t, 3H) 0.90 (t, 3H)The structural formula is shown below (a dashed line in the formula represents a conjugated structure).

1608-26-0, 1608-26-0 N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine 15355, achiral-phosphine-ligands compound, is more and more widely used in various fields.

Reference£º
Patent; Kanto Denka Kogyo Co., Ltd.; US2009/23954; (2009); A1;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1608-26-0,N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine,as a common compound, the synthetic route is as follows.

General procedure: A solution of methyl iodide (1.14 g, 8 mmol) was added dropwise for 1 min to the stirringmixture of tertiary phosphine (4 mmol) in anhydrous tetrahydrofuran (16 mL) at roomtemperature. After the mixture was stirred at room temperature for 12 h, the mixture wasevaporated in vacuo. The residue was washed with ether, and the precipitate was dried invacuo for 12 h at 40 C to give corresponding quaternary phosphonium iodide as a whitepowder.

1608-26-0, As the paragraph descriping shows that 1608-26-0 is playing an increasingly important role.

Reference£º
Article; Aoyagi, Naoto; Furusho, Yoshio; Endo, Takeshi; Tetrahedron Letters; vol. 54; 51; (2013); p. 7031 – 7034;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1608-26-0,N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine,as a common compound, the synthetic route is as follows.

The ligand precursor HP(OCH2CHi-PrNH)2 (2S,8S)-2,8-isopropyl-4,6-dioxa-1,9-diaza-5lambda5-phosphaspiro[4.4]nonane 1 was obtained using the general procedure described in the literature [9] A mixture of P(NMe2)3 (1.14?cm3, 6.27?mmol) and (S)-(+)-2-amino-3-methyl-butanol (CH3)2CHCH(NH2)CH2OH (0.31?g, 12.6?mmol) and 6?cm3 of toluene was placed in a round-bottomed flask equipped with a magnetic stirrer and a reflux condenser, and then heated gradually to 100?C over 2?h with gentle argon purging. The progress of the reaction was monitored by GC-MS analyses. The crude product (white solid) was purified by recrystallization from hexane in a freezer providing crystals suitable for X-ray analysis. Yield: 1.14?g (78%). Anal. Calc. for C10H23N2O2P: C, 51.27; H, 9.90; N, 11.96 Found: C, 50.82; H, 9.78; N, 11.6%; 1H NMR (CD2Cl2) major epimer 1a: delta 0.80, 0.89 (12H, d, 3J(H, H)?=?7?Hz, CH3), 1.45 (2H, m, CH), 2.87 (4H, m, CH, NH), 3.33 (2H, ddd, 2J(H, H)?=?8.9?Hz, 3J(H, H)?=?5.7?Hz, 3J(P, H)?=?10.00?Hz, CH2), 3.77 (2H, ddd, 2J(H, H)?=?8.9?Hz, 3J(H, H)?=?6.3?Hz, 3J(P, H)?=?11.36?Hz, CH2), 6.74 (1H, d 1J(P, H)?=?741.1?Hz, PH); minor epimer 1b: delta 0.84, 0.90 (12H, d, 3J(H, H)?=?7?Hz, CH3), 1.52 (2H, m, CH), 2.87 (4H, m, CH, NH), 3.48 (2H, ddd, 2J(H, H)?=?8.9?Hz, 3J(H, H)?=?4.9?Hz, 3J(P, H)?=?11.45?Hz, CH2), 3.69 (2H, ddd, 2J(H, H)?=?8.9?Hz, 3J(H, H)?=?6.5?Hz, 3J(P, H)?=?9.71?Hz, CH2), 6.76 (1H, d 1J(P, H)?=?727.3?Hz, PH) 31P {1H} NMR (CD2Cl2) delta – 53.73 (minor signal), -54.16 (major signal) ppm; IR numax(nujol)/cm-1 658vs, 953vs, 988vs, 1050vs, 1156?m nu(C-O-P), 2347?s 2360?s nu(P-H), 3324?s, nu(N-H); ESI-MS: m/z calcd for [M?+?H]+ 236.14 found 236.14; Deltaepsilon223?=?-0.43, 1608-26-0

1608-26-0 N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine 15355, achiral-phosphine-ligands compound, is more and more widely used in various fields.

Reference£º
Article; Skar?y?ska, Anna; Gniewek, Andrzej; Inorganica Chimica Acta; vol. 483; (2018); p. 248 – 251;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

1608-26-0, N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a mixture of (S)-3,3′-Dibenzyl-5,5′,6,6′-tetramethyl-1,1′-biphenyl-2,2′-diol24 (0.42 g, 1.00 mmol) in toluene (5 mL) was added hexamethylphosphorous triamide (248 mg, 1.50 mmol) under nitrogen. The resulting mixture was stirred at 80 C for 17 h. The solvent was evaporated under reduced pressure to afford a gel-like product, which was further purified by column chromatography on silica gel (pretreated with 1% NEt3 in hexanes) using hexanes/EtOAc (19/1) as the eluent to give (R)-MPN-Lf (0.32 g, 65%) as a white solid: mp 110.0-112.0 C; [alpha]D22 -176.2 (c 0.5, CH2Cl2); 1H NMR (400 MHz, CDCl3) delta 1.94 (s, 3H), 2.01 (s, 3H), 2.22 (s, 3H), 2.23 (s, 3H), 2.52 (s, 3H), 2.55 (s, 3H), 3.70 (d, J=15.2 Hz, 1H), 4.17 (m, 1H), 6.86 (s, 1H), 6.91 (s, 1H), 7.28 (m, 10H); 31P NMR (121.5 MHz, CDCl3) delta 140.8; HRMS (EI) calcd for C24H26NO2P [M]+ 391.1701, found 391.1703 (Delta=+0.5 ppm)., 1608-26-0

As the paragraph descriping shows that 1608-26-0 is playing an increasingly important role.

Reference£º
Article; Chien, Chih-Wei; Shi, Ce; Lin, Chi-Feng; Ojima, Iwao; Tetrahedron; vol. 67; 35; (2011); p. 6513 – 6523;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

1608-26-0, N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Tris(dimethylamino)phosphine (1.64 g, 10 mmol) was added drop-wise to a stirred solution of methanol (0.32 g, 10 mmol) andCCl4 (1.77 g, 11.5 mmol) in dry CH2Cl2 (20 mL) cooled at 30 C.Then, 10 mL of distilled water was added and the reaction mixturewas allowed to proceed at room temperature for 2 h. Organic phasewas decanted and extracted with water (2 30 mL). Aqueousphases were collected, washed with Et2O and decanted to give anaqueous solution of methoxytris(dimethylamino)phosphonium chloride CH3OP(NMe2)3Cl., 1608-26-0

1608-26-0 N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine 15355, achiral-phosphine-ligands compound, is more and more widely used in various fields.

Reference£º
Article; Mechria, Ali; Dridi, Sana; Msaddek, Moncef; Inorganica Chimica Acta; vol. 427; (2015); p. 173 – 177;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1608-26-0,N,N,N’,N’,N”,N”-Hexamethylphosphinetriamine,as a common compound, the synthetic route is as follows.

General procedure: A mixture of the aminobenzamidine 1 (5.0 mmol) andtris (dimthylamino) phosphine (5.0 mmol) dissolved in anhydroustoluene (10 mL) were heated under reflux for 48 h.After evaporating the solvent in vacuum, the resulting solidproduct was recrystallized from CCl4 (2b, 2d) or alternativelythe obtained oil (2a, 2c) was purified by columnchromatography using silica gel (60-120 mesh) with ethylacetate: petroleum ether (4 : 6) as eluant.2a: N,N-dimethyl-4-(propylimino)-3,4-dihydro-1,3,2-benzodiaza-phosphorin-2(1H)-amineYield : 70%, brown viscous oil. IR (FTIR, nu (cm-1)): nu(C=N) = 1634; nu (NH) = 3319. 1H NMR (CDCl3+DMSO-d6,delta (ppm)): delta = 0.80 (t, 3H, 3JH-H = 6 Hz, CH3-CH2); 1.20 (m,2H, 3JH-H = 6.3 Hz, CH3-CH2); 2.45 (d, 3JHP = 6 Hz, N-CH3);2.47 (d, 3JHP = 6 Hz, N-CH3); 2.90 (t, 2H, 3JH-H = 6.3 Hz, NCH2);5.20(broad s, 2H, NH); 6.50-7.70(m, 4H, Harom). 13CNMR (CDCl3+DMSO-d6, delta (ppm)): 14.90 (CH3-CH2); 29.0(CH3-CH2); 34.10 (C=N-CH2); 34.25 (N-CH3); 36.26 (NCH3);114.90; 122.20; 128.90; 130.50; 132.90; (Carom);133.51 (Carom-N-P); 153.86 (P-N-C=N-CH2). 31P NMR(CDCl3+ DMSO-d6, delta (ppm)): 0.29. Calcd. C12H19N4P : %C= 57.60 % H = 7.60 % N = 22.40; Found: %C = 57.59 % H= 7.65 % N = 22.39., 1608-26-0

The synthetic route of 1608-26-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Hichri, Sarra; Abderrahim, Raoudha; Letters in Organic Chemistry; vol. 13; 4; (2016); p. 289 – 292;,
Phosphine ligand
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate