The synthetic route of 285984-25-0 has been constantly updated, and we look forward to future research findings.
Related Products of 285984-25-0, These common heterocyclic compound, 285984-25-0, name is 3-(tert-Butyl)-1-(p-tolyl)-1H-pyrazol-5-amine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Preparation 38 5-fert-butyl-2- g-tolyl-2i7-pyrazol-3-ylVcarbamic acid. 2.2.2-trichloro-ethyl ester Add a saturated solution OfNa2CO3 (2.4 L) to a solution of 5-tert-butyl-2-/>-tolyl-2.ff-pyrazol-3- ylamine (400 g, 1.74 mol) in THF (8L) and cool the mixture to 0 C. Then dropwise add 2, 2, 2- trichloroethyl chloroformate (406.77 g, 1.92 mol) and stir the mixture at 0 C for 2 hours. Extract the reaction mixture with ethyl acetate (3 x 6.5L), dry over anhydrous magnesium sulfate and concentrate. Dissolve the solid in a minimal amount of ethyl acetate and add an excess of hexanes to precipitate. Collect the solid by filtration and dry to obtain the title compound as an off white solid (586 g, 83% yield). 1H NMR (400 MHz, CDCl3) delta 7.34 (d, 2H), 7.29 (d, 2H), 6.78 (bs, IH), 6.41 (bs, IH), 4.81 (s, 2H), 2.41 (s, 3H), 1.34 (s, 9H). MS(ES+): m/? = 406.1 [M+H].
The synthetic route of 285984-25-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ELI LILLY AND COMPANY; WO2007/53394; (2007); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics