Synthetic Route of 2468-56-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2468-56-6 as follows.
3) Synthesis of 6-trifluoroacetamido-1-hexyne To a solution of sodium hydride (60% oil, 2.55 g, 63.6 mol) in DMF (50 ml), trifluoroacetamide (8.99 g, 79.6 mmol) was added portionwise as about 10 portions with ice cooling. Subsequently, a solution of 6-iodo-1-hexyne (3.31 g, 15.9 mmol) in DMF (15 ml) was added to the reaction mixture. The reaction mixture was stirred at room temperature for four hours. The reaction mixture was added with saturated aqueous ammonium chloride (100 ml) and ether (100 ml) for extraction. The ether layer was dried over magnesium sulfate, and concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (eluent; hexane-ethyl acetate mixed solvent) to afford 2.0 g of 6-trifluoroacetamido-1-hexyne (yield; 65.4%). Melting point: 41.0-42.5 C. 1H-NMR (270 MHz, CDCl3) delta ppm: 1.53-1.80 (m, 4H, -CH2(CH2)2-), 1.98 (t, 1H, J=2.7 Hz, H-CC-), 2.26 (dt, 2H, J=2.5, 6.7 Hz, CC-CH2-), 3.41 (q, 2H, J=6.8 Hz, CH2-N), 6.48 (brs, 1H, NHTfa)
According to the analysis of related databases, 2468-56-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; The Institute of Physical and Chemical Research; US6265569; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com