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: Phosphorus triamides 10a, 10b (5.2 mmol) in 5 cm3 of dryTHF were added in one portion to a mixture of 0.8 g azide1 (3.9 mmol) and 2 cm3 dil. EtOH (1:1) in 10 cm3 THF.The reaction mixture was stirred at r.t. for &6 h (TLC).The solvent was evaporated to dryness; the residue waswashed several times with light petroleum (40-60 C), andcrystallized from the proper solvent to give 13a and 13b,respectively.N00-(3-Cyano-4,5,6,7-tetrahydro-1-benzothien-2-yl)-N,N,N?,N?-tetramethylphosphoric triamide(13a, C13H21N4OPS)Pale yellow crystals; yield: 0.97 g (79.6 %); m.p.: 165 C(MeCN); IR (KBr): v = 3325 (NH), 2205 (CN), 1232 (P=O,bonded) cm-1; 1H NMR (500.7 MHz, CDCl3): d = 1.91,2.32 (2 m, 4 9 2H, 4 H2C-hexyl), 2.45 (d, 3JPH = 9.4 Hz,2 9 6H, (Me2N)2P), 11.21 (br, 1H, HN) ppm; 13C NMR(125.4 MHz, CDCl3): d = 150.6 (d, 2JPC = 28.3 Hz, C-NH), 136.1, 130.2 (C=C-hexyl), 113.7 (CN), 87.3 (C-CN),35.5 (d, 2JPC = 13.5 Hz, (Me2N)2P), 26.4, 26.2, 23.5, 21.8(CH2-hexyl) ppm; 31P NMR (200.7 MHz, CDCl3):d = 34.7 ppm; MS (EI, 70 eV): m/z (%) = 311 (45)[M?-1], 285 (34) [M?-27 (H ? CN)], 150 (100) [M?-162 (H ? CN ? C4H12N2OP)]., 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; Abdou, Wafaa M.; Ganoub, Neven A.; Sabry, Eman; Monatshefte fur Chemie; vol. 147; 3; (2016); p. 619 – 626;,
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