Day: August 17, 2020

13689-19-5, Tricyclohexylphosphine oxide is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2. Conversion of Tricyclohexylphosphine Oxide to Tricyclohexylphosphine Hydrochloride and Tricyclohexylphosphine; The apparatus used was a 250 ml flask with Teflon paddle stirrer, thermometer, unimmersed gas introduction tube with rotameter and excess pressure release valve (0.1 bar), a reflux cooler with cryostat and downstream dry ice cooler and an NaOH scrubbing tower. The reflux condenser was cooled to -15 C. The flask was initially charged with 8.0 g (0.027 mol) of tricyclohexylphosphine oxide in 60 ml of anhydrous toluene at room temperature, and the phosgene introduction was commenced. The initially clear colorless solution became cloudy immediately and an exothermic reaction set in, which could be controlled by throttling the phosgene introduction such that the temperature of the reaction mixture did not exceed 38 C. In addition, gas evolution set in. The phosgene introduction was continued until the gas evolution had ended (11.1 g; 0.112 mol of phosgene). Subsequently, the reaction mixture was stirred for another 30 minutes, while the temperature fell to 25 C. To remove excess phosgene, the mixture was heated to 40 C. with introduction of nitrogen for 240 minutes, and then further nitrogen was introduced at room temperature overnight for complete removal of phosgene. After adding 50 ml of toluene and stirring for 30 minutes, the flask contents (130 g) were transferred to a miniautoclave in a glove box under argon, and the autoclave was purged twice with 150 bar of nitrogen and then twice with 150 bar of hydrogen. The reaction mixture was heated to 160 C. with stirring and 100 bar of hydrogen were injected. After 48 hours, within which the pressure fell to 97 bar, the mixture was cooled and decompressed. The white flaky precipitate formed was filtered off under argon and washed twice with 10 ml of toluene each time. After the solvent had been removed under reduced pressure, 7.4 g (86% of theory) of tricyclohexylphosphine hydrochloride were obtained as a white solid.31P NMR (1H-coupled) (145 MHz; toluene-d8): delta=28.00 (d, JP-H=440 Hz).Elemental analysis (dihydrochloride): C18H35Cl2PCalculated: C, 60.8; H, 10.5; P, 8.7.Found: C, 61.1; H, 10.2; P, 8.4.

The synthetic route of 13689-19-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Basf SE; US2010/137643; (2010); 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.13689-20-8,Cyclohexyldiphenylphosphine oxide,as a common compound, the synthetic route is as follows.

General procedure: To a solution of tertiary phosphine oxides 2 (0.4mmol) in CH2Cl2 (2mL) was added oxalyl chloride (0.4mmol) dropwise at room temperature under an argon atmosphere. After 30min, HEH (1mmol) was added to the mixture in one portion as well as TEA (3mmol). The mixture was stirred for another 2h at 40C, and then diluted with H2O (10mL). The resulting mixture was extracted with CH2Cl2 repeatedly. The extracts were dried (anhydrous Na2SO4) and evaporated. The crude product was purified by column chromatography on silica gel using ethyl acetate/petroleum ether to afford the pure product.

13689-20-8 Cyclohexyldiphenylphosphine oxide 83664, achiral-phosphine-ligands compound, is more and more widely used in various.

Reference£º
Article; Zhang, Tong-Xin; Zhang, Wei-Xi; Luo, Mei-Ming; Chinese Chemical Letters; vol. 25; 1; (2014); p. 176 – 178;,
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.

Tris(dimethylamino)phosphine (2.29g, 14mmol) was added drop-wise to a stirred solution of 2-methylprop-2-en-1-ol (1g, 14mmol) and CCl4 (2.46g, 16mmol) in dry CH2Cl2 (30mL) cooled at-30C. Then, 15mL of distilled water was added and the reaction mixture was allowed to proceed at room temperature for 2h. Organic phase was decanted and extracted with water (2¡Á40mL). Aqueous phases were collected, washed with Et2O and decanted to give an aqueous solution of methallyloxyphosphonium chloride. After the addition of KPF6 (3.68g, 20mmol) in 10mL of water, an immediate precipitate was formed. The mixture was filtered and the crude product was washed with Et2O and dried under vacuum. Recrystallization from a mixture of chloroform: Et2O solution afforded salt 2 as a white solid. Yield: 4.15g (78%). IR [nu cm-1]: 836 (PF6-). 1H NMR (300MHz, CDCl3): 1.78 (s, 3H, CH3-allyl); 2.76 (d, 18H, (CH3)2N); 4.54 (d, 2H, CH2-O); 5.01 (s, 1H, CH2); 5.08 (s, 1H, CH2). 13C NMR (75.47MHz, CDCl3): 18.7 (CH3-allyl); 36.7 (CH3-N); 71.9 (CH2-O); 114.3 (CH2); 137.7 (C).

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

Reference£º
Article; Dridi, Sana; Mechria, Ali; Msaddek, Moncef; Journal of Organometallic Chemistry; vol. 772-773; (2014); p. 217 – 221;,
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

166330-10-5, (Oxybis(2,1-phenylene))bis(diphenylphosphine) is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: To a solution of HPDPH (35.5mg, 0.16mmol) in THF (6mL) was added NaH (60percent, 6.51mg, 0.16mmol) to form a yellow solution. After stirring for 10min, CuCl (15.87mg, 0.16mmol) and XANTPhos (92.85mg, 0.16mmol) were added. The yellow resulting solution was stirred overnight and filtered. The filtrate was layered with hexane to give yellow crystals which were suitable for an X-ray diffraction study.

The synthetic route of 166330-10-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Wang, Ya-Ping; Hu, Xiao-Hui; Wang, Yi-Fan; Pan, Jun; Yi, Xiao-Yi; Polyhedron; vol. 102; (2015); p. 782 – 787;,
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

1079-66-9, Chlorodiphenylphosphine is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Under nitrogen protection,1L three bottles,From 50 g of 4-bromo-N, N-dimethylaniline,7 g of magnesium turnings and 400 ml of anhydrousTHF to produce Grignard reagent,Refluxed for 10 hours, reduced to room temperature,2.9 g of tetrakis (triphenylphosphine) palladium was added,Stirred for 3 hours,61 g of diphenylphosphonium chloride was added dropwise at room temperature,The reaction was refluxed for 8 hours.And the mixture was added dropwise to the reaction solution under ice-water bath200 mL of saturated aqueous ammonium chloride was quenched,Liquid separation, the organic phase solution,Add methanol crystallization,And filtered to obtain 74 g of white 4- (N, N-dimethylamino) diphenylphosphine benzene,Yield 96percent.

1079-66-9 Chlorodiphenylphosphine 66180, achiral-phosphine-ligands compound, is more and more widely used in various.

Reference£º
Patent; Panjin Gelin Kaimo Technology Co., Ltd.; Rao, Zhihua; Gong, Ningrui; (12 pag.)CN105859774; (2016); A;,
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

434336-16-0, (Oxybis(2,1-phenylene))bis(dicyclohexylphosphine) is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A 50 ml three-necked flask equipped with a stirring reflux device was charged with 1 mmol of 2-diethylphosphine aniline,1.3 mmol of o-methoxybenzyl alcohol, 1 mmol2-dicyclohexylphosphine oxide, 1 mmol RuCl2 (PPh3) 3, 1.1 mmol potassium hydroxide, 20 ml benzene and heating at a temperature of 100 C for 18 h under a nitrogen atmosphere,After cooling and filtering, the resulting solid was recrystallized from a mixed solvent of CH 2 Cl 2 and petroleum ether to give product 15 in a yield of 80%.

As the paragraph descriping shows that 434336-16-0 is playing an increasingly important role.

Reference£º
Patent; Luoyang Normal College; Li Hongmei; Xu Chen; Zu Enpu; Xiao Zhiqiang; Han Xin; (12 pag.)CN104804048; (2017); B;,
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

166330-10-5, (Oxybis(2,1-phenylene))bis(diphenylphosphine) is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of anhydrous FeCl3 (100 mg; 0.615 mmol)in 20 mL acetonitrile, a solution of the ligand DPEphos (662mg; 1.23 mmol) in 30 mL acetonitrile was added. The reaction mixture was refluxed under continuous flow of N2 for1h. The color of the solution turned dark brown from yellow.After cooling the reaction mixture, the solvent was evaporated and the resultant solid mass was washed several timeswith ether and hexane. Finally, after drying under vacuum, adark brown compound was obtained which was recrystallized from acetonitrile. Yield: 88percent; Anal. Calcd. forC72H56O2P4Cl3Fe: C, 69.78; H, 4.55; Fe, 4.51. Found: C,69.47; H, 4.58; Fe, 4.49, Selected peak assignments in MSESIm/z (percent): 1242 (10), [M-Cl+K]+; 1164 (40), [MPh+2H]2+; 539 (100), [DPEphos]+; Selected IR frequencies(cm-1, KBr): 3060 (C-H), 1481, 1438 (C=C); 1102 (C-O-C);545 (Fe-P); Far IR (Nujol): 387, 339, 314(Fe-Cl); UV-Vis(CH3CN), max (nm): 229, 272, 360.

166330-10-5 (Oxybis(2,1-phenylene))bis(diphenylphosphine) 4285986, achiral-phosphine-ligands compound, is more and more widely used in various.

Reference£º
Article; Sahu, Debojeet; Banik, Biplab; Borah, Malabika; Das, Pankaj; Letters in Organic Chemistry; vol. 11; 9; (2014); p. 671 – 676;,
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

50777-76-9, 2-(Diphenylphosphino)benzaldehyde is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A mixture of p-toluenesulfonic acid (10 mg), 2-(diphenylphosphino)benzaldehyde (282 mg, 0,974 mmol) and3-amino-2-(S)-1-hydroxyethyl)-3H-quinazolin-4-one(100 mg, 0,487 mmol) in ethanol (10 mL) and heated at120 ¡ãC for 12 h. The reaction was cooled and analyzed by TLC [ethylacetate:hexane/1:5]. The solvent was evaporatedunder reduced pressure until dryness and the residue wasdissolved in CH2Cl2.The solution was washed with NaHCO3followed by H2Oand the organic phase was dried withNa2SO4.The crude product, obtained by evaporation of thesolvent, was purified by chromatography on silica gel using1:9 ethylacetate:hexane as an eluent. Yield 101 mg (44percent),m.p.: 130?131 ¡ãC (dec.). 1H NMR (400.2 MHz, CDCl3):delta(ppm) 9.88 (d, 1H, JPH = 5.8 Hz, HC = N), 8.12 (m, 2H,ArCH), 7.52 (m, 2H, ArCH), 7.44?7.21 (m, 12H, ArCH),6.84 (m, 2H, ArCH), 4.84 (m, 1H, CH), 4.35 (s, OH), 1.34(d, 3H, J = 6.4 Hz, CH3).13C NMR (100.6 MHz, CDCl3):delta (ppm) 165.5 (d, JPC = 19.2 Hz, N = CH), 158.7?121.6(Ar), 65.4 (CH), 22.1 (CH3). 31P{1H} NMR (162.0 MHz,CDCl3):delta (ppm) ? 15.35 (s). FTIR (KBr, cm?1): 3451 (OH);1687 (C = O); 1607 (C = N); 1435 (P-Ph). Anal. calcd. forC29H24N3O2P:C, 72.95; H, 5.07; N, 8.80percent. Found: C, 73.33;H, 5.29; N, 8.47percent.

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Reference£º
Article; Y?lmaz, Mustafa Kemal; Kele?, Mustafa; Transition Metal Chemistry; vol. 43; 3; (2018); p. 285 – 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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.13885-09-1,2-(Diphenylphosphino)biphenyl,as a common compound, the synthetic route is as follows.

A suspension of copper(I) iodide (0.042 g, 0.22 mmol) and dpbp (0.149 g, 0.44 mmol) in 15 mL ofCH2Cl2 was stirred for 3 h at room temperature to form a white precipitate. The precipitate was filteredoff and purified by recrystallization from CH2Cl2/aectonitrile to give colorless crystals (Yield: 0.160 g,84.2percent). 1H NMR (400 M, CDCl3) delta: 7.44?7.26 (m, 26H, m,p-Ph + ?PC6H4?), 7.09?6.99 (m, 12H, o-Ph). 13CNMR (100 M, CDCl3) delta: 147.87, 147.67, 140.24, 140.16, 134.31, 134.17, 133.45, 132.17, 131.81, 131.07,130.71, 130.14, 129.90, 128.93, 128.69, 127.93, 127.26 (Ar?C). 31P NMR (240 M, CDCl3) delta ?10.16 (s). Anal.Calcd for C48H38CuIP2: C, 66.48; H, 4.42. Found: C, 66.50; H, 4.40. MS (MALDI-TOF): m/z Calcd for [M?I]+,739.1745, found 739.1874.

As the paragraph descriping shows that 13885-09-1 is playing an increasingly important role.

Reference£º
Article; Qi, Lei; Li, Qian; Hong, Xiao; Liu, Li; Zhong, Xin-Xin; Chen, Qiao; Li, Fa-Bao; Liu, Qian; Qin, Hai-Mei; Wong, Wai-Yeung; Journal of Coordination Chemistry; vol. 69; 24; (2016); p. 3692 – 3702;,
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

1070663-78-3, Dicyclohexyl(2′,4′,6′-triisopropyl-3,6-dimethoxy-[1,1′-biphenyl]-2-yl)phosphine is a chiral-phosphine-ligands compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 0848 A mixture of 2-chloro-7-(1,3-dimethyl-1H-pyrazol-4-yl)-1,5-naphthyridine (20 mg), 3-isopropylisoxazole-5-amine (10 mg), tris(dibenzylideneacetone)dipalladium(0) (4 mg), 2-(dicyclohexylphosphino)-3,6-dimethoxy-2′,4′,6′-triisopropyl-1,1′-biphenyl (4 mg), sodium tert-butoxide (11 mg), and 1,4-dioxane (0.6 mL) was stirred at 140 C. for 30 minutes using a microwave reaction apparatus. The reaction mixture was cooled to room temperature, the insolubles were filtered off, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate-methanol, chloroform-methanol, NH silica), thereby obtaining N-(7-(1,3-dimethyl-1H-pyrazol-4-yl)-1,5-naphthyridin-2-yl)-3-isopropylisoxazole-5-amine (0.8 mg) as a pale yellow solid. 1H-NMR (DMSO-d6) delta: 8.88 (1H, d, J=2.0 Hz), 8.22 (3H, d, J=9.9 Hz), 7.31 (1H, d, J=8.6 Hz), 6.70 (1H, s), 6.55 (1H, s), 3.85 (3H, s), 3.03-2.94 (1H, m), 2.43 (3H, s), 1.29 (6H, d, J=6.6 Hz). MS m/z (M+H): 349.

As the paragraph descriping shows that 1070663-78-3 is playing an increasingly important role.

Reference£º
Patent; FUJIFILM Corporation; FURUYAMA, Hidetomo; KURIHARA, Hideki; TERAO, Takahiro; NAKAGAWA, Daisuke; TANABE, Shintaro; KATO, Takayuki; YAMAMOTO, Masahiko; SEKINE, Shinichiro; MASHIKO, Tomoyuki; INUKI, Shinsuke; UEDA, Satoshi; US2015/322063; (2015); 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