Electric Literature of 1450754-38-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1450754-38-7 name is 3-(But-3-yn-1-yl)-3-(2-iodoethyl)-3H-diazirine, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
K2CO3 (0.207g, 1.5 mmoL) and L3 (0.248g, 1.0 mmoL) were added orderly to a solution of phenol (0.113g, 1.2 mmoL) in DMF (10mL). The reaction mixture was stirred at 50C for 16h and monitored by TLC. The reaction was quenched by adding H2O (5mL). The crude product was exacted into EtOAc (3×10mL). The combined organic layers were washed with brine (10mL), and dried over Na2SO4 and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by flash column chromatography giving NP as colorless oil (171mg, yield 80%). 1H NMR (300MHz, CDCl3) delta 7.34-7.28 (m, 2H), 7.01-6.95 (m, 1H), 6.94-6.88 (m, 2H), 3.85 (t, J=6.2Hz, 2H), 2.13-2.06 (m, 2H), 2.01 (t, J=2.6Hz, 1H), 1.91 (t, J=6.2Hz, 2H), 1.80-1.73 (m, 2H). 13C NMR (75MHz, CDCl3) delta 158.4, 129.5, 121.1, 114.5, 82.8, 69.2, 62.4, 33.0, 32.7, 26.7, 13.3. Purity: 97.13% by (0.01M KH2PO4 solution: MeOH=15: 85).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-(But-3-yn-1-yl)-3-(2-iodoethyl)-3H-diazirine, and friends who are interested can also refer to it.