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. 39806-90-1 name is 4-Iodo-1-methyl-1H-pyrazole, 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. 39806-90-1
A mixture of 5-((1,2,3,5,6,7-hexahydro-s-indacen-4-yl)amino)-1-((2-(trimethylsilyl)- ethoxy)methyl)-1H-1,2,4-triazole-3-thiol (Intermediate B9) (300 mg, 521.57 mumol, 1 eq), 4-iodo-1-methyl-1H-pyrazole (108 mg, 521.57 mumol, 1 eq), CuI (198 mg, 1.04 mmol, 2 eq) and N,N’-dimethylethane-1,2-diamine (919 mg, 10.43 mmol, 20 eq) in dioxane (4 mL) was stirred at 70C under N2 atmosphere for 2 hours. The reaction mixture was poured into water (10 mL) and extracted with ethyl acetate (3 ¡Á 10 mL). The organic layers were dried over anhydrous Na2SO4, filtered and concentrated in vacuum. The residue was purified by prep-TLC (SiO2, petroleum ether: ethyl acetate, 1:1) to give the title compound (200 mg, 79.44% yield) as a yellow solid.1H NMR (400 MHz, CDCl3) d 7.62 (s, 1H), 7.58 (s, 1H), 6.95 (s, 1H), 6.18 (s, 1H), 5.28 (s, 2H), 3.90 (s, 3H), 3.59 (t, 2H), 2.88 (t, 4H), 2.67 (t, 4H), 2.06-2.03 (m, 4H), 0.96- 0.92 (t, 2H), 0.02 (s, 9H).LCMS: m/z 483.1 (M+H)+(ES+).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Iodo-1-methyl-1H-pyrazole, and friends who are interested can also refer to it.